Synthesis and crystal structure of a novel multimodal ligand, 6,6’-bis(2-(di(pyridin-2-yl)methylene)-1- methylhydrazinyl)-2,2’-bipyridine, and its copper(I) complex, ${[Cu_ 3L_ 2](PF_ 6)_ 3.3H_ 2O}$
Synthesis and crystal structure of a novel multimodal ligand, 6,6’-bis(2-(di(pyridin-2-yl)methylene)-1- methylhydrazinyl)-2,2’-bipyridine, and its copper(I) complex, ${[Cu_ 3L_ 2](PF_ 6)_ 3.3H_ 2O}$
The single crystal X-ray structure of the novel multimodal ligand 6,6’-bis(2-(di(pyridin-2-yl)methylene)- 1-methylhydrazinyl)-2,2’-bipyridine, $C _{34}H _{28}N _{10}$ (L), was determined at 120 (2) K. The ligand possesses a centre of symmetry that generates a planar bipyridyl core with the hydrazone substituents in a transgeometry. The di-2-pyridyl moieties at either terminus of the molecule twist out of the plane (52.90 and 56.32 ˚A). The crystal structure comprises 2-dimensional ribbons that stack about each other so as to optimise van der Waals interactions and packing efficiency. Studies of the coordination properties of the novel multimodal ligand with copper(I) show that 2 ligand strands wrapped around the copper(I) having a preference for tetrahedral geometry to furnish a supramolecular self-assembled of a double-stranded tri-nuclear helical complex, ${[Cu_ 3L_ 2](PF_ 6)_ 3.3H_ 2O}$ (1), as revealed by the ESI-MS, and further characterised by $^ 1 H$-NMR, UV-Vis, and FT-IR spectra.
___
- 1. Maurya, M. R.; Khurana, S.; Schulzke, C.; Rehder, D. Eur. J. Inorg. Chem. 2001, 779-788.
- 2. Pelagatti, P.; Bacchi, A.; Carcelli, M.; Costa, M.; Fruhauf, H.-W.; Goubitz, K.; Pelizzi, C.; Triclistri, M.; Vrieze, K. Eur. J. Inorg. Chem. 2002, 439-446.
- 3. Giorgi, G.; Ponticelli, F.; Savini, L.; Chiasserini, L.; Pellerano, C. J. Chem. Soc., Perkin Trans. 2000, 2259-2264.
- 4. Sengul, A.; Wang, J. W.; Coles, S. J. Polyhedron 2009, 28, 69-76.
- 5. Shu, M. H.; Sun, W. U.; Duan, C. Y.; Fu, Y. J.; Zhang, W. J.; Tang, W. X. J. Chem. Soc., Dalton Trans. 1999, 729-734.
- 6. Ziessel, R. Coord. Chem. Rev. 2001, 195-223.
- 7. Bakir, M.; Hassan, I.; Green, O. J. Coord. Chem. 2006, 59 , 1953-1962.
- 8. Suni, V.; Kurup, M. R. P.; Nethaji, M. Polyhedron 2007, 26 , 3097-3102.
- 9. Yorke, J.; Dent, C.; Decken, A.; Xia, A. Inorg. Chem. Commun. 2010, 13, 54-57.
- 10. Schmitt, J. L.; Stadler, A. M.; Kyritsakas, N.; Lehn, J. M. Helv. Chim. Acta. 2003, 86, 1598-1624.
- 11. COLLECT. Nonius BV, Delft, The Netherlands. 1998.
- 12. Sheldrick, G.M. SHELX-97, A Program for Crystal Structure Solution and Refinement, University of Gottingen, Germany, 1997.
- 13. Sheldrick, G. M. SADABS V2.10. Bruker AXS Inc., Madison, Wisconsin, USA. 2007.
- 14. Otwinowski, Z.; Minor, W. Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by Carter Jr, C. W. and Sweet, R. M. New York: Academic Press, 1997, 307-326.
- 15. Spek, A. L. J. Appl. Cryst. 2003, 36, 7-13.
- 16. Bakir, M.; Brown, O. J. Mol. Struct. 2002, 641, 183-191.
- 17. Bachechi, F.; Buruni, A.; Galassi, R.; Pietroni, B. R.; Ricciutelli, M. Inorg. Chim. Acta. 2004, 357, 4349-4357.
- 18. Stadler, A.-M.; Kyritsakas, N.; Vaughan, G.; Lehn, J.-M. Chem. Eur. J. 2007, 13, 59-68.
- 19. Horn, C. J.; Blake, A. J.; Champness, N. R.; Garau, A., Lippolis, V.; Wilson, C.; Schr¨oder, M. Chem. Commun 2003, 312-313.
- 20. Thompson, A. M. W. C.; Blandford, I.; Redfearn, H.; Jeffery, J. C.; Ward, M. D. J. Chem. Soc., Dalton Trans., 1997, 2661-2665.
- 21. Constable, E. C. Nature 1990, 346, 314-315.
- 22. Araki, K.; Fuse, M.; Kishii, N.; Shiraishi, S. Bulletin of the Chemical Society of Japan. 1992, 65, 1220-1224.
- 23. Nakamoto, K. Infrared Spectra of Inorganic and Coordination Compounds, J ohn Wiley & Sons, New York, London, 1963.
- 24. Coates, J. Encyclopaedia of Analytical Chemistry, Interpretation of Infrared Spectra, A Practical Approach,Meyers, A.R., Eds. John Wiley & Sons Ltd, Chichester, 2000.
- 25. Braibanti, A.; Dallavalle, F.; Pellinghelli, M.A. and Leporati, E. Inorg. Chem. 1968, 7, 1430-1433.
- 26. Young, A. G.; Hanton, L. R. Coord. Chem. Rev. 2008, 252, 1346-1386.