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Journal of Structural Chemistry

, Volume 49, Issue 6, pp 1098–1103 | Cite as

X-ray diffraction structural investigation of two hafnium(IV) complexes with dipivaloylmethane

  • K. V. Zherikova
  • I. A. Baidina
  • N. B. Morozova
  • N. V. Kuratieva
  • I. K. Igumenov
Article

Abstract

Synthesis and single crystal X-ray diffraction study of hafnium(IV) dipivaloylmethanate Hf(dpm)4 and chloro-tris-(dipivaloylmethanato)hafnium(IV) Hf(dpm)3Cl have been carried out. Crystal data: a = 22.6606(5) Å, b = 11.3990(4) Å, c = 19.8513(7) Å, β = 106.458(1)°, Pc, Z = 4, d calc = 1.231 g/cm3, R = 0.075 for C44H76HfO8; a = 10.6376(13) Å, b = 10.6701(10) Å, c = 19.4400(22) Å, α = 74.970(3)°, β = 75.672(3)°, γ = 61.725(2)°, P-1, Z = 2, d calc = 1.366 g/cm3, R = 0.031 for C33H57ClHfO6. The structures are molecular and are built from discrete mononuclear complexes joined by van der Waals interactions. Disordering of carbon atoms preserving at low temperature is observed for the compound Hf(dpm)4. It has been found out that the structure contains two crystallographically unique complexes of hafnium(IV) with central atoms coordinated with eight oxygen atoms of four dipivaloylmethane ligands, bond lengths Hf-O fall within 2.084–2.222 Å, the distances Hf...Hf between the molecules are 10.07–13.87 Å. In Hf(dpm)3Cl the hafnium atom is seven-coordinated with six oxygen atoms of three β-diketonate ligands and one chlorine atom, the distances Hf-O fall within 2.087–2.179 Å, the lengths of the bond Hf-Cl for two crystallographically independent molecules Hf(1) and Hf(2) are 2.466 Å and 2.442 Å, respectively.

Keywords

hafnium(IV) β-diketonates synthesis single crystal X-ray diffraction mononuclear complex mass-spectrometry study 

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References

  1. 1.
    K. V. Zherikova, N. B. Morozova, N. V. Kuratieva, et al., J. Struct. Chem., 46, No 6, 1039–1046 (2005).CrossRefGoogle Scholar
  2. 2.
    K. V. Zherikova, N. B. Morozova, E. V. Peresypkina, et al., ibid., 47, No. 3, 570–574 (2006).CrossRefGoogle Scholar
  3. 3.
    K. V. Zherikova, N. B. Morozova, I. A. Baidina, et al., ibid., 47, No. 1, 82–86 (2006).CrossRefGoogle Scholar
  4. 4.
    Bruker AXS Inc. (2004). APEX2 (Version 1.08), SAINT (Version 7.03), SADABS (Version 2.11) and SHELXTL (Version 6.12). Bruker Advanced X-ray Solutions, Madison, Wisconsin, USA.Google Scholar
  5. 5.
    G. I. Spijksma, H. J. M. Bouwmeester, D. H. A. Blank, et al., Inorg. Chem., 45, No. 13, 4938 (2006).CrossRefGoogle Scholar
  6. 6.
    M. Jardin, Y. Gao, J. Guery, and C. Jacoboni, Acta Crystallogr., C51, 2230 (1995).CrossRefGoogle Scholar

Copyright information

© Pleiades Publishing, Ltd. 2008

Authors and Affiliations

  • K. V. Zherikova
    • 1
  • I. A. Baidina
    • 1
  • N. B. Morozova
    • 1
  • N. V. Kuratieva
    • 1
  • I. K. Igumenov
    • 1
  1. 1.A. V. Nikolaev Institute of Inorganic ChemistryRussian Academy of Sciences, Siberian DivisionNovosibirskRussia

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