Bulletin of the Korean Chemical Society

  • 제15권2호
  • /
  • Pages.150-153
  • /
  • 1994
  • /
  • 0253-2964(pISSN)
  • /
  • 1229-5949(eISSN)
대한화학회 (Korean Chemical Society)
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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)
  • 발행 : 1994.02.20
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초록

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.

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참고문헌

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