Journal of the Korean Chemical Society (대한화학회지)

Korean Chemical Society (대한화학회)
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Synthesis and Characterization of Tetranuclear Molybdenum(Ⅵ) Complexes with Butylamidoxime Derivatives

부틸아미드옥심 유도체의 몰리브덴(Ⅵ) 사핵 착물의 합성과 성질

  • Roh, Soo-Gyun (Department of Chemistry, Kyungpook National University) ;
  • Oh, Sang Oh (Department of Chemistry, Kyungpook National University)
  • 로수균 (경북대학교 자연과학대학 화학과) ;
  • 오상오 (경북대학교 자연과학대학 화학과)
  • Published : 19950700
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Abstract

The tetranuclear complexes, $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X= n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X = CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$ have been synthesized by the reactions of monomeric and polynuclear complexes with isobutyl-, butyl- and thiomethylacetamidoxime. The prepared complexes were identified by elemental analysis, infrared, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The structure of complex ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$ was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z=2, final R=0.026 for 2951($F_0>3s(F_0)$). This complex is composed of a planar cyclic $[Mo_4({\mu}-O)_4]$ and two ${\mu}_4$-amidoximate.

배위자인 이소부틸, 노르말 부틸 및 메틸티오아세트아미드옥심과 출발 물질인 단핵 및 다핵 착물과의 반응에서 $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X=n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X=CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$을 합성하였다. 합성한 착물은 원소분석, 적외선 및 핵자기공명에 의해 구조를 규명하였다. 얻은 착물중 ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$은 X-선 단결정 회절에서 결정구조를 밝혔고, 얻은 데이타는 Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z = 2이었고, 회절강도 2951개($F_0>3s(F_0)$)에 대한 최종 신뢰도 인자는 0.026이었다. 이 착물의 구조는 평면상의 환형$[Mo_4({\mu}-O)_4]$과 두 개의 ${\mu}_4$-아미드옥시메이트로 구성되어 있다.

Keywords

References

  1. Heteropoly and Isopolyoxometalates Pope, M. T.
  2. Angew. Chem., Int. Ed. Engl. v.30 Pope, M. T.;Muller, A.
  3. J. Am. Chem. Soc. v.112 Neumann, R.;Abu-Guim, C.
  4. J. Chem. Soc., Chem. Commun. El Ali, B.;Bregeault, J.-M.;Mercier, J.;Martin, C.;Convert, O.
  5. Inorg. Chem. v.28 Chambers, R. C.;Hill, C. L.
  6. Angew. Chem., Int. Ed. Eng. v.37 Renneke, C. A.;Hill, C. L.
  7. New J. Chem. v.17 Salles, L.;Aubry, C.;Robert, F.;Chottard, R.;Thouvenot, R.;Ledon, H.;Bregeault, J.-M.
  8. J. Am. Chem. Soc. v.113 Mansuy, D.;Bartoli, J.-F.;Battioni, P.;Lyon, D. K.;Finke, R. G.
  9. Inorg. Chem. v.23 McCarron, E. M.;Staley, H. H.;Sleight, W.
  10. J. Am. Chem. Soc. v.105 McCarron, E. M.;Harlow, R. L.
  11. Inorg. Chem. v.28 Kang, H.;Liu, S.;Shaikh, S. N.;Nicholson, T.;Zubieta, J.
  12. J. Am. Chem. Soc. v.111 Chen, Q.;Ma, L.;Liu, S.;Zubieta, J.
  13. Acta Cryst. v.C39 Wilson, A. J.;Robinson, W. T.;Wilkins, C. J.
  14. Inorg. Chem. v.28 Ma, L.;Liu, S.;Zubieta, J.
  15. Polyhedron v.9 Liu, S.;Ma, L.;McGowy, D.;Zubieta, J.
  16. Inorg. Chem. v.29 Chen, Q.;Zubieta, J.
  17. J. Am. Chem. Soc. v.114 Khan, M. I.;Chen, Q.;Goshorn, P.;Hope, H.;parkin, S.;Zubieta, J.
  18. Inorg. Chem. v.31 Chen, G.;Zubieta, J.
  19. J. Chem. Soc., Chem. Commun. Adams, A.;Klemperer, W. G.;Liu, R.
  20. J. Am. Chem. Soc. v.101 Day, V. W.;Fredrich, M. F.;Klemperer, W. G.;Liu, R.-S.
  21. Polyhedron v.8 Chen, Q.;Liu, S.;Zhu, H.;Zubieta, J.
  22. Inorg. Chem. v.25 Shaikh, S. N.;Zubieta, J.
  23. J. Chem. Soc., Chem. Commun. Kang, H.;Zubieta, J.
  24. Inorg. Chem. v.24 Hsieh, T.-C.;Zubieta, J.
  25. Polyhedron v.5 Hsieh, T.-C.;Zubieta, J.
  26. Inorg. Chim. Acta v.164 Chen, Q.;Liu, S.;Zubieta, J.
  27. Inorg. Chem. v.27 Bank, S.;Liu, S.;Shaikh, S. N.;Sun, X.;Zubieta, J.;Ellis, P. D.
  28. J. Am. Chem. Soc. v.114 Du, Y. H.;Rheingold, A. L.;Maatta, E. A.
  29. Inorg. Chem. v.23 McCarron, E. M.;Whitney, J. F.;Chase, D. B.
  30. Prog. Inorg. Chem. v.39 Pope, M. T.
  31. Coord. Chem. Rev. v.114 Chen, Q.;Zubieta, J.
  32. Doctoral Dissertation: Pierre et Marie Curie University Roh, S. -G.
  33. Inorg. Chem. v.15 Chen, G. J. J.;MacDonald, J. W.;Newton, W. E.
  34. Inorg. Chem. v.26 Nagasawa, A.;Tanka, H. K.;Miyoshi, M.;Saito, K.
  35. Inorg. Synth. v.29 Grimes, R. N.;Chakravorty, A.
  36. Inorg. Synth. v.27 Hur, N. H.;Klemperer, W. G.;Wang, R.-C.
  37. Angew. Chem., Int. Ed. Engl. v.28 Gouzerh, P.;Jeannin, Y.;Proust, A.;Robert, F.
  38. Chem. Rev. v.62 Eloy, F.;Lenaers, R.
  39. Calculations were performed with: Structure Determination System, Molen Enraf-Nonius
  40. J. Chem. Soc., Chem. Comm. Chilou, V.;Gouzerh, P.;Jeannin, Y.;Robert, F.
  41. Inorg. Chim. Acta v.178 Chilou, V.;Gouzerh, P.;Jeannin, Y.;Knobler, C. B.
  42. J. Chem. Soc., Dalton, Trans. Proust, A.;Gouzerh, P.;Robert, F.
  43. J. Am. Chem. Soc. v.101 Day, V. W.;Fredrich, M. F.;Klemperer, W. G.;Liu, R.-S.
  44. Inorg. Chem. v.19 Barkigia, K. M.;Rajkovic-Blazer, L. M.;Pope, M. T.;Prince, E.;Quicksall, C. O.
  45. Angew. Chem. Int. Ed. Engl. v.25 Buchlotz, R.;Mattes, R.
  46. Inorg. Chem. v.9 Stomberg, R.;Trysberg, L.;Larking, I.
  47. Polyhedron v.5 Hursthouse, M. B.;Short, R. L.;Piggot, B.;Tucker, A.;Wong, S. F.
  48. J. Am. Chem. Soc. v.109 Day, V. W.;Klemperer, W. G.;Schwartz, C.