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Journal of Chemical Crystallography

, Volume 36, Issue 4, pp 249–254 | Cite as

Crystal Structure of bis(O,O′-neopentylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width145pt depth0pt}\hspace*{-147pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and bis(O,O′-hexylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width164pt depth0pt}\hspace*{-166pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2

  • A. L. Bingham
  • J. E. Drake
  • K. Saraswat
  • M. Nirwan
  • M. B. Hursthouse
  • M. E. Light
  • R. Ratnani
Article

Purple crystals of bis(O,O′-neopentylene dithiophosphato)nickel(II), Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and bis(O,O′-hexylene dithiophosphato)nickel(II), Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width83.5pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 were obtained by layering benzene solutions of the complexes with ether and maintaining the samples at room temperature. The molecular structures of Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width84pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 were determined by single-crystal X-ray diffraction. Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 crystallizes as monoclinic in the space group P21/c with cell parameters a = 7.051(2) Å, b = 6.453(2) Å, c = 19.686(6) Å, β = 99.45(3)°, V = 883.6(5) Å−3, Z = 2, R = 0.0251, R w = 0.0599. Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width84pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 crystallizes as triclinic in the space group P-1 with cell parameters a = 8.394(5) Å, b = 11.070(5) Å, c = 12.124(5) Å, α = 71.287(5)°, β = 76.227(5)°, γ = 88.319(5)°, V = 1035.0(9) Å−3, Z = 2, R = 0.0655, R w = 0.1545. In both complexes the environment around nickel is distorted square planar.

KEY WORDS:

Synthesis structure nickel neopentylene hexylene dithiophosphate 

Notes

Acknowledgments

One of us (M.N.) is grateful to CSIR, New Delhi for financial support. M.B.H. Thanks to the UK Engineering and Physical Sciences Council for support of the X-ray facilities at Southampton University. J.E.D. thanks the University of Windsor for financial support.

References

  1. 1.
    Wasson, J.R.; Woltermann, G.M.; Stoklosa, H.J. Top. Curr. Chem. 1973, 35, 65.Google Scholar
  2. 2.
    Micu-Semeniuc, R.; Dumitrescu-Silaghi, L.; Haiduc, I. Inorg. Chim. Acta 1979, 33, 281.CrossRefGoogle Scholar
  3. 3.
    Black, L.F.; Graddon, D.P. Inorg. Chim. Acta 1978, 30, 327.CrossRefGoogle Scholar
  4. 4.
    Pilipenko, A.T.; Melnikova, N.V.; Strashko, V.V. Koord. Khim. 1979, 5, 1372.Google Scholar
  5. 5.
    Fayyaz, M.U.; Grant, M.W. Aust. J. Chem. 1978, 31, 1439.CrossRefGoogle Scholar
  6. 6.
    Hynes, M.J.; Brannick, P.F. J. Chem. Soc., Chem. Commun. 1977, 24, 942.CrossRefGoogle Scholar
  7. 7.
    Micu-Semienuic, R.; Silaghi-Dumitrescu, L.; Chirila, N.; Haiduc, I. Rev. Roumaine Chim. 1980, 25, 1025.Google Scholar
  8. 8.
    Zhumadilov, E.K.; Markova, E.I.; Nefedov, V.I. Koord. Khim. 1978, 4, 997.Google Scholar
  9. 9.
    Bhasin, C.P.; Srivastava, G.; Mehrotra, R.C. Inorg. Chim. Acta 1983, 77, L131.CrossRefGoogle Scholar
  10. 10.
    Bhasin, C.P.; Srivastava, G.; Mehrotra, R.C. Inorg. Chim. Acta 1987, 128, 69.CrossRefGoogle Scholar
  11. 11.
    Bhasin, C.P.; Srivastava, G.; Mehrotra, R.C. Inorg. Chim. Acta 1987, 131, 195.CrossRefGoogle Scholar
  12. 12.
    So, H.; Lin, Y.C.; Huang, G.S.; Chang, S.T. Wear 1993, 166, 17–26.CrossRefGoogle Scholar
  13. 13.
    Mikhailov, V.V.; Kokhannov, Y.V.; Kazaryan, K.; Matreeva, E.N.; Kozodoi, A. Plast. Massy 1970, 9, 23–24.Google Scholar
  14. 14.
    Gupta, A.K.S.; Srivastava, R.C.; Parma, S.S. Can. J. Chem. 1967, 45, 2993.CrossRefGoogle Scholar
  15. 15.
    Hoskins, B.F.; Tiekink, E.R.T. Acta Crystallogr. Sect. C: Crystal Struct. Commun. 1985, 41, 322.CrossRefGoogle Scholar
  16. 16.
    Jian, F.; Xiao, H.; Li, Y.; Jiao, K. J. Chem. Crystallogr. 2003, 33, 705.CrossRefGoogle Scholar
  17. 17.
    Yu, Y.; Zhu, D.; Liu, S.; Lin, C.; Xu, Z.; Gou, S.; You, X. Jiegou Huaxue 1990, 9, 73.Google Scholar
  18. 18.
    Hao, Q.; Fun, H.K.; Chantrapromma, S.; Razak, I.A.; Jian, F.; Yang, X.; Lu, L.; Wang, X. Acta Crystallogr., Sect. C: Crystal Struct. Commun. 2001, 57, 717.CrossRefGoogle Scholar
  19. 19.
    Hao, Q.; Jian, F.; Wang, X.; Razak, I.A.; Shanmuga, S.R.S.S.; Fun, H.K. Acta Crystallogr., Sect. C: Crystal Struct. Commun. 2001, 57, 160.CrossRefGoogle Scholar
  20. 20.
    Huang, X.Y.; Xiong, R.G.; You, X.Z. Acta Crystallogr., Sect. C: Crystal Struct. Commun. 1995, 51, 2261.CrossRefGoogle Scholar
  21. 21.
    Bhasin, C.P.; Srivastava, G.; Mehrotra, R.C.; Hitchcock, P.B. Inorg. Chim. Acta 1989, 11, 164.Google Scholar
  22. 22.
    Chauhan, H.P.S.; Bhasin, C.P.; Srivastava, G.; Mehrotra, R.C. Phosphor. Sulphur 1983, 15, 99.CrossRefGoogle Scholar
  23. 23.
    Duisenberg, A.J.M. J. Appl. Cryst. 1992, 25, 92.CrossRefGoogle Scholar
  24. 24.
    Sheldrick, G.M. SADABS version 2.10; University of Gottingen: Germany 2003. Google Scholar
  25. 25.
    Sheldrick, G.M. Acta Cryst. A 1990, 46, 467.CrossRefGoogle Scholar
  26. 26.
    Farrugia, L.J. J. Appl. Cryst. 1999, 32, 837.CrossRefGoogle Scholar
  27. 27.
    Sheldrick, G.M. SHELXL97, Structure Determination Software; University of Gottingen: Germany, 1997.Google Scholar
  28. 28.
    Machala, V.; Travnicek, Z.; Sindelar, Z.; Kvitek, L. Trans. Met. Chem. 2000, 25, 715–719.CrossRefGoogle Scholar
  29. 29.
    Shun'ichior, O.; Fernando, Q. Inorg. Chem. 1967.Google Scholar
  30. 30.
    Drake, J.E.; Khasrou, L.N.; Mislankar, A.G.; Ratnani, R. Polyhedron 2000, 19, 407.CrossRefGoogle Scholar
  31. 31.
    Shetty, P.S.; Fernando, Q. J. Am. Chem. Soc. 1970.Google Scholar

Copyright information

© Springer Science+Business Media, Inc. 2005

Authors and Affiliations

  • A. L. Bingham
    • 1
  • J. E. Drake
    • 2
  • K. Saraswat
    • 3
  • M. Nirwan
    • 3
  • M. B. Hursthouse
    • 1
  • M. E. Light
    • 1
  • R. Ratnani
    • 3
  1. 1.Department of ChemistryUniversity of Southampton, HighfieldSouthamptonUnited Kingdom
  2. 2.Department of Chemistry and BiochemistryUniversity of WindsorWindsorCanada
  3. 3.Department of Pure and Applied ChemistryM.D.S. UniversityAjmerIndia

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