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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 15, Number 2
BKCSDE 15(2)
February 20, 1994 

Preparation and Structure of Re(≡NC6H5)(CO)(PPh3)Cl3
Young-Woong Kim, June-Ho Jung, Soon W. Lee*
By treating mer, trans-Re(=NC6H5)(PPh3)2Cl3, Ⅰ, with 5 atm of CO at room temperature for 52 h, fac-Re(=NC6H5)(CO)(PPh3)Cl3, 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 P21/n with cell parameters a=9.740 (2) Å, b=16.210 (5) Å, c=16.192 (6) Å, β=97.50 (2)°, and Z=4. Least-squares refinement of the structure led to a R(Rw) factor of 0.030 (0.036) for 2878 unique reflections of I>3σ(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) Å and the bond angle of Re-N-C(Ph) became smaller from 172.6 (6) to 167.0 (2)°, 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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