Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
권호 표지
DOI QR코드

DOI QR Code

Preparation and Structure of Re$({\equiv}NC_6H_5)(CO)(PPh_3)Cl_3$

  • Young-Woong Kim (Department of Chemistry, Sung Kyun Kwan University) ;
  • Jun-Ho Jung (Department of Chemistry, Sung Kyun Kwan University) ;
  • Soon W. Lee (Department of Chemistry, Sung Kyun Kwan University)
  • Published : 1994.02.20
Download PDF
⟨ Previous Next ⟩

Abstract

By treating mer, trans-Re(${\equiv}NC_6H_5)(PPh_3)_2Cl_3$, Ⅰ, with 5 atm of CO at room temperature for 52 h, fac-Re(${\equiv}NC_6H_5)(CO)(PPh_3)Cl_3$, Ⅱ, was obtained as dark green precipitates in 81% yield. The crystal structure of Ⅱ was determined through X-ray diffraction. Ⅱ crystallizes in the monoclinic system, space group $P2_1/n$ with cell parameters a=9.740 (2) ${\AA}$, b=16.210 (5) ${\AA}$, c=16.192 (6) ${\AA}$, ${\beta}$=97.50 $(2)^{\circ}$, and Z=4. Least-squares refinement of the structure led to a R$(R_w)$ factor of 0.030 (0.036) for 2878 unique reflections of I>3${\sigma}(I)$ and for 241 variables. In comparison to the starting material Ⅰ, the bond distance of Re-N became longer from 1.726 (6) to 1.736 (5) ${\AA}$ and the bond angle of Re-N-C(Ph) became smaller from 172.6 (6) to 167.0 $(2)^{\circ}$, indicating that the Re-N bond in Ⅱ is weakened and has a less triple-bond character than that in Ⅰ.

Keywords

References

  1. Metal-Ligand Multiple Bonds Nugent, W. A.;Mayer, J. M.
  2. Comprehensive Coordination Chemistry v.2 Chisholm, M. H.;Rothwell, I. P.;Wilkinson, G.(ed.);Gillard, R. D.(ed.);McCleverty, J. A.(ed.)
  3. Coord. Chem. Rev. v.31 Nugent, W. A.;Haymore, B. L.
  4. Inorga. Chim. Acta v.18 Cenini, S.;La Monica, G.
  5. J. Chem. Soc. Commun. Maata, E. A.;Du, Y.;Rheingold, A. L.
  6. lnorg. Chem. v.26 Bakir, M.;Fanwick, P. E.;Walton, R. A.
  7. J. Am. Chem. Soc. v.114 Gray, S. D.;Smith, D. P.;Bruck, M. A.;Wigley, D. E.
  8. Catal. Today v.10 Perot, G.
  9. J. Am. Chem. Soc. v.113 Glueck, D. S.;Wu, J.;Hollande, F. J.;Bergman, R. G.
  10. Inorg. Chem. Acta v.29 La Monica, G.;Cenini, S.
  11. J. Chem. Soc. Chatt, J.;Garforth, J. D.;Johnoson, N. P.;Rowe, G. A.
  12. J. Chem. Soc. Dalton La Monica, G.;Cenini, S.
  13. J. Chem. Soc., Chem. Commun. Chatt, J.;Dilworth, J. R.
  14. Acta Cryst. v.C40 Forellini, E.;Casellato, U.
  15. Inorganic Chemistry(4th ed.) Huheey, J. E.;Keiter, E. A.;Keiter, R. L.