Tetraphenylborate adducts of lead(II) co-ordinated by imidazole-functionalized 1,4,7-triazacyclononanes: crystal and molecular structures

Abstract

The new functionalized macrocycles 1-(1-methylimidazol-2-ylmethyl)-1,4,7-triazacyclononane, L¹, 1,4-bis(1-methylimidazol-2-ylmethyl)-1,4,7-triazacyclononane, L², and 1,2-bis[4,7-bis(1-methylimidazol-2-ylmethyl)-1,4,7-triazacyclonon-1-yl]ethane, L³, have been synthesized. The reaction of hydrated lead(II) acetate with these compounds in the presence of sodium tetraphenylborate afforded the complexes [PbL¹Cl(BPh₄)]·0.5MeCN, [PbL²(BPh₄)]BPh₄ and [Pb₂L³(BPh₄)₂][BPh₄]₂·4MeCN which were characterized in the solid state by elemental analyses and X-ray crystallography. The lead(II) atoms are co-ordinated by the nitrogens of the macrocyclic ring, by the nitrogen donor(s) of the pendant imidazole group(s) and, in the complex with the L¹ ligand, also by a chlorine atom. In each of the three complexes a phenyl group of a tetraphenylborate anion lies at close contact distance from the lead and completes its co-ordination.

References

1. M. J. Hynes and B. Jonson, Chem. Soc. Rev., 1997, 26, 133; K. Abu-Dari, F. E. Hahn and K. N. Raymond, J. Am. Chem. Soc., 1990, 112, 1519.
2. D. L. Reger, J. E. Collins, A. L. Rheingold, L. M. Liable-Sands and G. P. A. Yap, Inorg. Chem., 1997, 36, 345; J. Parr, A. T. Ross and A. M. Z. Slawin, J. Chem. Soc., Dalton Trans., 1996, 1509; A. Andres, A. Bencini, A. Carachalios, A. Bianchi, P. Dapporto, E. Garcia-España, P. Paoletti and P. Poli, J. Chem. Soc., Dalton Trans., 1993, 3507; K. Abu-Dari, T. B. Karpishin and K. N. Raymond, Inorg. Chem., 1993, 32, 3052; D. L. Reger, M. F. Huff, A. L. Rheingold and B. S. Haggerty, J. Am. Chem. Soc., 1992, 114, 579; K. Wieghardt, M. Kleine-Boymann, B. Nuber, J. Weiss, L. Zsolnai and G. Hutter, Inorg. Chem., 1986, 25, 1647; N. W. Alcock, E. H. Curzon and P. Moore, J. Chem. Soc., Dalton Trans., 1984, 2813.
3. M. Di Vaira, F. Mani and P. Stoppioni, J. Chem. Soc., Dalton Trans., 1997, 1375; 1994, 3739; G. de Martino Norante, M. Di Vaira, F. Mani, S. Mazzi and P. Stoppioni, J. Chem. Soc., Dalton Trans., 1992, 361; M. Di Vaira, B. Cosimelli, F. Mani and P. Stoppioni, J. Chem. Soc., Dalton Trans., 1991, 331.
4. M. Di Vaira, M. Guerra, F. Mani and P. Stoppioni, J. Chem. Soc., Dalton Trans., 1996, 1173.
5. T. J. Atkins, J. E. Richman and W. F. Oettle, Org. Synth., 1978, 58, 86; K. Wieghardt, W. Schmid, B. Nuber and I. Weiss, Chem. Ber., 1978, 112, 2220.
6. R. G. Jones, J. Am. Chem. Soc., 1949, 71, 383.
7. M. Di Vaira, F. Mani and P. Stoppioni, Inorg. Chim. Acta, 1998, 273, 151.
8. K. Wieghardt, I. Tolksdorf and W. Herrmann, Inorg. Chem., 1985, 24, 1230.
9. A. Buttafava, L. Fabbrizzi, A. Perotti, G. Poggi and B. Seghi, Inorg. Chem., 1986, 25, 1456.
10. DIFABS, N. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158.
11. SIR 92, A. Altomare, M. C. Burla, M. Camalli, G. Cascarano, C. Giacovazzo, A. Guagliardi and G. Polidori, J. Appl. Crystallogr., 1994, 27, 435.
12. G. M. Sheldrick, SHELXL 93, Program for Crystal Structure Refinement, University of Göttingen, 1993.
13. PARST, M. Nardelli, J. Appl. Crystallogr., 1995, 28, 659.
14. C. K. Johnson, ORTEP II, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, TN, 1976.
15. R. Hoffmann, Angew. Chem., Int. Ed. Engl., 1982, 21, 711.
16. CACAO, C. Mealli and D. M. Proserpio, J. Chem. Educ., 1990, 67, 399.
17. A. G. Gash, P. F. Rodesiler and E. L. Amma, Inorg. Chem., 1974, 13, 2429.
18. J. L. Lefferts, K. C. Molloy, M. B. Hossain, D. van der Helm and J. J. Zuckerman, Inorg. Chem., 1982, 21, 1410 and refs. therein.