Skip to main content
Log in

Formation of a samarium alkoxide–aryloxide complex containing a novel butterfly framework: X-ray crystal structures of Sm4(μ3-O-i-Pr)3(μ2-O-i-Pr)4(O-i-Pr)2(O-2,6-i-Pr2C6H3)3(THF) and [Ti(O-i-Pr)2(O-2,6-i-Pr2C6H3) (μ-O-i-Pr)]2

  • Published:
Journal of Chemical Crystallography Aims and scope Submit manuscript

Abstract

Reaction of a 1:1 mixture of Sm[N(SiMe3)2]3 and Ti(O-i-Pr)4 with three equivalents of 2,6-di-iso-propylphenol, followed by crystallization from hexane/THF, leads to isolation of the tetranuclear samarium alkoxide Sm43-O-i-Pr)32-O-i-Pr)4(O-i-Pr)2(O-2,6-i-Pr2C6H3)3(THF) (1), in addition to the dimeric titanium alkoxide [Ti(O-i-Pr)2(O-2,6-i-Pr2C6H3)(μ-O-i-Pr)]2 (2). 1 crystallizes in the space group \(P\bar 1\) while 2 crystallizes in space group P21/c. Cell parameters for 1: a = 15.928(6), b = 17.677(7), c = 18.99(1) Å, α = 113.24(3), β = 94.99(4), γ = 109.59(2)°, V = 4477(4) Å3, D calc = 1.350 Mg/m3, and Z = 2. Cell parameters for 2: a = 25.336(2), b = 12.082(1), c = 15.570(2) Å, β = 96.510(8)°, V = 4735.4(8) Å3, D calc = 1.129 mg/m3, and Z = 4.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Similar content being viewed by others

References

  1. (a) Bettahar, M.M.; Costentin, G.; Savary, L.; Lavalley, J.C. Appl. Catal. A 1996, 145, 1. (b) Tokura, Y. Curr. Opin. Solid State Mater. Sci. 1998, 3, 175. (c) Negas, T.; Davies, P.K. Ceram. Trans. 1995, 53, 179. (d) Dimza, V.I. Ferroelectrics 1996, 188, 53.

  2. Hubert-Pfalzgraf, L.G. New J. Chem. 1995, 19, 727.

    Google Scholar 

  3. (a) Martin, M.J.; Mendiola, J.; Zaldo, C. Ferroelectr. Lett. Sect. 1997, 22, 101. (b) Soo Paik, D.; Prasadarao, A.V.; Komarneni, S. S. Mater. Lett. 1997, 33, 97. (c) Alvarez-Fregoso, O. J. Appl. Phys. 1997, 81, 1387. (d) Calzada, M.L.; Sirera, R.; Ricote, J.; Pardo, L. J. Mater. Chem. 1998, 8, 111.

  4. Takata, T.; Furumi, Y.; Shinohara, K.; Tanaka, A.; Hara, M.; Kondo, J.N.; Domen, K. Chem. Mater. 1997, 9, 1063.

    Google Scholar 

  5. (a) Nakamura, T.; Shan, Y.J.; Sun, P-H.; Inaguma, Y.; Itoh, M. Solid State Ionics 1998, 108, 53. (b) Sun, P.H.; Nakamura, T.; Shan, Y.J.; Inaguma, Y.; Itoh, M. Ferroelectrics 1997, 200, 93.

  6. Satheesh, V.; Murugavel, P.; Murthy, V.R.K.; Viswanathan, B. Mater. Sci. Eng. B 1997, B48, 202.

    Google Scholar 

  7. (a) Ohsato, H.; Mizuta, M.; Ikoma, T.; Onogi, Y.; Nishigaki, S.; Okuda, T. J. Ceram. Soc. Jpn. 1998, 106, 178. (b) Rawn, C.J.; Birnie, D.P., III; Bruck, M.A.; Enemark, J.H.; Roth, R.S. J. Mater. Res. 1998, 13, 187. (c) Sekar, M.M.A.; Patil, K.C. Mater. Sci. Eng. B 1996, B38, 273.

  8. (a) Caulton, K.G.; Hubert-Pfalzgraf, L.G. Chem. Rev. 1990, 90, 969. (b) Chandler, C.D.; Roger, C.; Hampden-Smith, M.J. Chem. Rev. 1993, 93, 1205.

  9. (a) Hubert-Pfalzgraf, L.G.; Daniele, S.; Bennaceur, A.; Daran, J-C.; Vaissermann, J. Polyhedron 1997, 16, 1223. (b) Daniele, S.; Hubert-Pfalzgraf, L.G.; Daran, J-C.; Halut, S. Polyhedron 1994, 13, 927.

  10. Moustiakimov, M.; Kritikos, M.; Westin, G. Acta Crystallogr. Sect. C 1998, 54, 29.

    Google Scholar 

  11. XSCANS and SHELXTL PCare products of Siemens Analytical X-ray Instruments, Inc., 6300 Enterprise Lane, Madison, Wisconsin 53719. SHELX-93 is a program for crystal structure refinement written by G.M. Sheldrick, (1993), Univ. of Go¨ttingen, Germany.

  12. R1 _ ___Fo___Fc__/ __Fo_ and R2w _ [_[w(F2o _ F2c )2]/_[w(F2o )2]]1/2. The parameter w _ 1/[ _2(F2o ) _ (0.0903*P)2].

  13. R1 _ ___Fo___Fc__/ __Fo_ and R2w _ [_[w(F2o _ F2c )2]/_[w(F2o )2]]1/2. The parameter w _ 1/[ _2(F2o ) _ (0.0559*P)2].

  14. For examples of lanthanide alkoxide complexes containingUOR, _2-OR and _3-OR ligands, see (a) Bradley, D.C.; Chudzynska, H.; Hammond, M.E.; Hursthouse, M.B.; Motevalli, M.; Ruowen, W. Polyhedron 1992, 11, 375. (b) Bradley, D.C.; Chudzynska, H.; Hursthouse, M.B.; Motevalli, M. Polyhedron 1991, 10, 1049. (c) Bradley, D.C.; Chudzynska, H.; Frigo, D.M.; Hammond, M.E.; Hursthouse, M.B.; Mazid, M.A. Polyhedron 1990, 9, 719. (d) Andersen, R.A.; Templeton, D.H.; Zalkin, A. Inorg. Chem. 1978, 17, 1962.

  15. Butcher, R.J.; Clark, D.L.; Gordon, J.C.; Watkin, J.G. J. Organomet. Chem. 1999, 577, 228.

    Google Scholar 

  16. Clark, D.L.; Gordon, J.C.; Huffman, J.C.; Watkin, J.G.; Zwick, B.D. Polyhedron 1996, 15, 2279.

    Google Scholar 

  17. Evans, W.J.; Drummond, D.K.; Hughes, L.A.; Zhang, H.; Atwood, J.L. Polyhedron 1988, 7, 1693.

    Google Scholar 

  18. Evans. W.J.; Ulibarri, T.A.; Ziller, J.W. Organometallics 1991, 10, 134.

    Google Scholar 

  19. Sirio, C.; Hubert-Pfalzgraf, L.G.; Bois, C. Polyhedron 1997, 16, 1129.

    Google Scholar 

  20. Evans, W.J.; Sollberger, M.S.; Hanusa, T.P. J. Am. Chem. Soc. 1988, 110, 1841.

    Google Scholar 

  21. Anwander, R.; Munck, F.C.; Priermeier, T.; Scherer, W.; Runte, O.; Herrmann, W.A. Inorg. Chem. 1997, 36, 3545.

    Google Scholar 

  22. Yunlu, K.; Gradeff, P.S.; Edelstein, N.; Kot, W.; Shalimoff, G.; Streib, W.E.; Vaartstra, B.A.; Caulton, K.G. Inorg. Chem. 1991, 30, 2317.

    Google Scholar 

  23. (a) Harlow, R.L. Acta Crystallogr. Sect. C 1983, 39, 1344. (b) Borgias, B.A.;Cooper, S.R.; Koh, Y.B.;Raymond, K.N. Inorg. Chem. 1984, 23, 1009. (c) Boyle, T.J.; Barnes, D.L.; Heppert, J.A.; Morales, L.; Takusagawa, F.; Connolly, J.W. Organometallics 1992, 11, 1112. (d) Boyle, T.J.; Alam, T.M.; Mechenbier, E.R.; Scott, B.L.; Ziller, J.W. Inorg. Chem. 1997, 36, 3293. (e) Fisher, J.; van der Sluys, W.G.; Huffman, J.C.; Sears, J. Synth. React. Inorg. Met.-Org. Chem. 1993, 23, 479.

  24. Barnhart, D.M.; Clark, D.L.; Gordon, J.C.; Huffman, J.C.; Watkin, J.G.; Zwick, B.D. Inorg. Chem. 1995, 34, 5416.

    Google Scholar 

  25. Boyle, T.J.; Alam, T.M.; Tafoya, C.J.; Scott, B.L. Inorg. Chem. 1998, 37, 5588.

    Google Scholar 

  26. Wu, Y-T.; Ho, Y-C.; Lin, C-C.; Gau, H-M. Inorg. Chem. 1996, 35, 5948.

    Google Scholar 

  27. Veith, M.; Mathur, S.; Huch, V. Inorg. Chem. 1997, 36, 2391.

    Google Scholar 

  28. Hubert-Pfalzgraf, L.G.; Machado, L.; Vaissermann, J. Polyhedron 1996, 15, 545.

    Google Scholar 

  29. Scott, B.L.; Watkin, J.G.; Young, K.J., submitted to J. Chem. Crystallogr.

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

Click, D.R., Scott, B.L. & Watkin, J.G. Formation of a samarium alkoxide–aryloxide complex containing a novel butterfly framework: X-ray crystal structures of Sm4(μ3-O-i-Pr)3(μ2-O-i-Pr)4(O-i-Pr)2(O-2,6-i-Pr2C6H3)3(THF) and [Ti(O-i-Pr)2(O-2,6-i-Pr2C6H3) (μ-O-i-Pr)]2. Journal of Chemical Crystallography 29, 921–929 (1999). https://doi.org/10.1023/A:1009530112983

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1009530112983

Navigation