An oxovanadium(IV) complex containing a pentacoordinate Schiff-base ligand: synthesis and crystal and molecular structure of N,N′-(3,3′-dipropylamine)bis (3-methoxysalicylideneiminato)oxovanadium(IV) dihydrate

  • Elmer C. Alyea
  • Terence D. Dee
  • George Ferguson
Article

Abstract

Crystals ofN,N′-(3,3′-dipropylamine)bis(3-methoxysalicylideneiminato) oxovanadium(IV) dihydrate are monoclinic, space groupP21/n (No. 14) with four molecules in the unit cell of dimensionsa=8.667(4),b=20.617(4),c=12.744(3) Å,β=91.48(3)°. The structure was solved by the heavy-atom method and refined by block diagonal least-squares calculations with anisotropic thermal parameters for nonhydrogen atoms.R=0.038 for 1457 reflections withI>3σ(I). This structure is the first reported for an oxovanadium(IV) complex involving complexation of a pentacoordinate Schiff-base ligand. The coordination polyhedron is based on a distorted octahedron. Three nitrogen and one oxygen atom from the ligand form an equatorial plane around vanadium with V-N(1) 2.096(4), V-N(2) 2.180(4), V-N(3) 2.088(4), V-O(2) 1.961(3) Å, and octahedral coordination is completed by the vanadyl oxygen [V-O(1) 1.617(3) Å] and the remaining ligand oxygen [V-O(3) 2,098(3) Å]. The relatively long V-O(1) distance correlates well with the low value ofv(V=O) of 919 cm−1. The molecules of the complex are linked by water molecules of crystallization to form infinite hydrogen-bonded chains parallel toa.

Keywords

Crystallization Vanadium Oxygen Atom Dihydrate Equatorial Plane 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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References

  1. Alyea, E. C., and Dee, T. D. (1984), to be published.Google Scholar
  2. Bersted, B. H., Belford, R. L., and Paul, I. C. (1968)Inorg. Chem. 7, 1557.Google Scholar
  3. Casey, A. T., and Thackeray, J. R. (1969)Aust. J. Chem. 22, 2459.Google Scholar
  4. Cotton, F. A., and Wilkinson, G. (1980)Advanced Inorganic Chemistry, 4th edn. (Interscience, New York), p. 715.Google Scholar
  5. Cromer, D. T., and Liberman, D. (1970)J. Chem. Phys. 53, 1891.Google Scholar
  6. Cromer, D. T., and Mann, J. B. (1968)Acta Cryst. A 24, 321.Google Scholar
  7. Fallon, G. D., and Gatehouse, B. M. (1976)Acta Cryst. B 32, 71.Google Scholar
  8. Ginsberg, A. P., Koubek, E., and Williams, H. J. (1966)Inorg. Chem. 5, 1657.Google Scholar
  9. Havinale, B. R., and Pujar, I. B. (1981)J. Inorg. Nucl. Chem. 43, 2689.Google Scholar
  10. Hazell, A. C. (1963)J. Chem. Soc., 5745.Google Scholar
  11. Hon, P. K., Bedford, R. L., and Pfluger, C. E. (1965)J. Chem. Phys. 43, 3111.Google Scholar
  12. Kalinnikov, V. T., Zelentsov, V. V., Kuzmicheva, O. N., and Aminov, T. C. (1970)RUSS. J. Inorg. Chem. 15, 341.Google Scholar
  13. Kierkegaard, P., and Longo, J. M. (1965)Acta Chem. Scand. 19, 1906.Google Scholar
  14. Larson, A. C., and Gabe, E. J. (1978)Computing in Crystallography, H. Schenkel al., eds. (Delft Univ. Press), pp. 81–89.Google Scholar
  15. Mathew, M., Carty, A. J., and Palenik, G. J. (1970)J. Am. Chem. Soc. 92, 3197.Google Scholar
  16. Ooi, S., Nishizawa, M., Matsumoto, K., Kuroya, H., and Saito, D. (1979)Bull. Soc. Chem. Jpn. 52, 452.Google Scholar
  17. Oughtred, R. E., Raper, E. S., Shearer, H. M. M. (1976)Acta Cryst. B 32, 82.Google Scholar
  18. Pasini, A., and Gullotti, M. (1974)J. Coord. Chem. 3, 319.Google Scholar
  19. Pasquali, M., Marchetti, F., Floriani, C., and Merlino, S. (1977)J. Chem. Soc. Dalton Trans., 139.Google Scholar
  20. Pasquali, M., Marchetti, F., Floriani, C., and Cesari, M. (1980)Inorg. Chem. 19, 1198.Google Scholar
  21. Patel, K. S., Kolawole, G. A., and Earnshaw, A. (1981)Inorg. Nucl. Chem. 43, 3107.Google Scholar
  22. Pettersen, R. C. (1969)Acta Cryst. B 25, 2527.Google Scholar
  23. Rastogi, D. K., Sahni, S. K., Rana, V. B., Dua, K., and Dua, S. K. (1979)J. Inorg. Nucl. Chem. 41, 21.Google Scholar
  24. Sacconi, L., and Bertini, I. (1966)J. Am. Chem. Soc. 88, 5180.Google Scholar
  25. Seibin, J. (1965)Chem. Rev. 65, 153.Google Scholar
  26. Stewart, R. F., Davidson, E. R., and Simpson, W. T. (1965)J. Chem. Phys. 42, 3175.Google Scholar
  27. Syamal, A. (1975)Coord. Chem. Rev. 16, 309.Google Scholar
  28. Syamal, A. (1978)Trans. Met. Chem. 3, 297.Google Scholar
  29. Theobald, F., and Galy, J. (1973)Acta Cryst. B 29, 2732.Google Scholar

Copyright information

© Plenum Publishing Corporation 1985

Authors and Affiliations

  • Elmer C. Alyea
    • 1
  • Terence D. Dee
    • 1
  • George Ferguson
    • 1
  1. 1.Department of ChemistryUniversity of GuelphGuelphCanada

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