Design and Characterization of Amino and Chloro Functionalized Rhombohedral Silsesquioxanes
A more rapid and a versatile synthetic approach for the preparation of polyhedral silsesquioxanes (POSS) by hydrolytic condensation of organosilicon monomers in the presence of a Pt catalyst was studied. The structural properties of POSS molecules were determined by X-ray powder diffraction analysis, yielding a rhombohedral unit cell with a = 11,52796Å and a = 94,9754° for octaaminopropyl-POSS, and a rhombohedral unit cell with a = 11,51421Å, a = 96,7214° for octachloropropyl-POSS. The activation energies were found to be 64.8, and 89.1 kJ/mol for octaaminopropyl-POSS and octachloropropyl-POSS, respectively. The products were also characterized by Fourier transform infrared spectroscopy, 1H and 13C nuclear magnetic resonance, differential thermal analysis, and thermogravimetric analysis.
Design and Characterization of Amino and Chloro Functionalized Rhombohedral Silsesquioxanes
A more rapid and a versatile synthetic approach for the preparation of polyhedral silsesquioxanes (POSS) by hydrolytic condensation of organosilicon monomers in the presence of a Pt catalyst was studied. The structural properties of POSS molecules were determined by X-ray powder diffraction analysis, yielding a rhombohedral unit cell with a = 11,52796Å and a = 94,9754° for octaaminopropyl-POSS, and a rhombohedral unit cell with a = 11,51421Å, a = 96,7214° for octachloropropyl-POSS. The activation energies were found to be 64.8, and 89.1 kJ/mol for octaaminopropyl-POSS and octachloropropyl-POSS, respectively. The products were also characterized by Fourier transform infrared spectroscopy, 1H and 13C nuclear magnetic resonance, differential thermal analysis, and thermogravimetric analysis.
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- F.J. Feher, D. Soulivong, A.G. Eklund, Chem. Commun. 399-400 (1998).
- F.J. Feher, D. Soulivong, F.Nguyen, Chem. Commun. 1279-1280 (1998).
- F.J. Feher, K.D. Wyndham, D.J. Knauer, Chem. Commun. 2393-2394 (1998).
- F.J. Feher, K.D. Wyndham, M.A. Scialdone, Y.Hamuro, Chem. Commun. 1469-1470 (1998).
- F.J. Feher, D. Soulivong, A.G. Eklund, K.D. Wyndham, Chem. Commun. 1185-1186 (1997).
- R.A. Mantz, P.F. Jones, K.P. Chaffe, J.D. Lichtenhan, J.W. Gilman, Chem. Mater. 8, 1250-1259 (1996).
- F.J. Feher, D. Soulivong, G.T. Lewis, J. Am. Chem. Soc. 119, 11323-11324 (1997).
- A. Lee, J.D. Lichtenhan, Macromolecules 31, 4970-4974 (1998).
- F.J. Feher, K.D. Wyndham, Chem. Commun. 323-324 (1998).
- A.N. Marui, C.C. Riccardi, Polymer Bulletin 45, 523-530 (2001).
- A. Sellinger, R.M. Laine, Chem. Mater. 8, 1592-1593 (1996).
- F.J. Feher, S.H. Phillips, J.W. Ziller, J. Am. Chem. Soc. 119, 3397-3398 (1997).
- C. Zhang, F. Babonneau, C.Bonhemme, R.M.Laine, C.L.Soles, H.A.Hristov, A.F. Yee, J. Am. Chem. Soc.
- , 8380-8391 (1998). 14. T. Kudo, M.S. Gordon, J. Am. Chem. Soc. 120, 11432-11438 (1998). 15. A. Sellinger, R.M. Laine, Macromolecules 29, 2327-2330 (1996). 16. T.S. Haddad, J.D. Lichtenhan, Macromolecules 29, 7302-7304 (1996). 17. A. Tsuchida, C. Bolln, F.G. Sernetz, H. Frey, R. M¨ulhaupt, Macromolecules 30, 2818-2824 (1997). 18. J.L. Hedrick, H.J. Cha, R.D. Miller, D.Y. Yoon, H.R. Brown, S. Srinivasan, R.D. Pietro, R.F. Cook, J.P.
- Hummel, D.P. Klaus, E.G. Liniger, and E.E. Simonyi Macromolecules 30, 8512-8515 (1997). 19. A. Lee, J.D. Lichtenhan, Macromolecules 31, 4970-4974 (1998). 20. B.R. Harkness, K.Takeuchi, M. Tachikawa, Macromolecules 31, 4798-4805 (1998). 21. D.P. Fasce, R.J.J. Williams, F. Mechin, J.P. Pascault, M.F. Llauro, R. Petiaud, Macromolecules 32, 4757- 4763 (1999). 22. J.Pyun, K. Matyjaszewski, Macromolecules 33, 217-220 (2000). 23. P. Eisenberg, R. Erra-Balsells, Y. Ishikawa, J.C. Lucas, A.N. Mauri, H. Nonami, C.C. Riccardi, R.J.J. Williams,
- Macromolecules 33, 1940-1947 (2000). 24. V. Chandrasekhar, R. Murugavel, A. Voigt, H.W. Roesky, H.G. Schmidt, M. Noltemeyer, Organometallics
- , 918-922 (1996). 25. A. Klemp, H.W. Roesky, H.G. Schmidt, H.S. Park, M. Noltemeyer, Organometallics 17, 5225-5227 (1998). 26. R. Duchateau, H.C.L. Abbenhuis, R.A. van Santen, S.K.H. Thiele, M.F.H. van Tol, Organometallics 17,
- 5224 (1998). 27. R. Duchateau, U. Cremer, R.J. Harmsen, S.I. Mohamud, H.C.L. Abbenhuis, R.A. van Santen, A. Meetsma,
- S.K.H. Thiele, M.F.H. van Tol, M. Kranenburg, Organometallics 18, 5447-5459 (1999). 28. R. Duchateau, R.A. van Santen, G.P.A. Yap, Organometallics 19, 809-816 (2000). 29. H.E. Kissinger, Anal. Chem. 29, 1702 (1957).