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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 15, Number 10
BKCSDE 15(10)
October 20, 1994 

 
Title
Preparation and Structure of Re(≡NC6H5)(PPh3)(PR3)Cl3, PR3=PMe3, P(OMe)3
Author
Young-woong Kim, June-ho Jung, Hee-sook Park, Soon W. Lee*
Keywords
Abstract
Reactions of mer, trans-Re(≡NC6H5)(PPh3)2Cl3, Ⅰ, with PMe3 and P(OMe)3 at room temperature, led to mer, trans-Re(≡NC6H5)(PPh3)(PMe3)Cl3, Ⅱ, and fac-Re(≡NC6H5)(PPh3)(P(OMe)3)Cl3, Ⅲ, respectively. The crystal structures of Ⅱ and Ⅲ were determined through X-ray diffraction. Ⅱ crystallizes in the orthorhombic system, space group Pna21 with cell parameters a=19.379(4) Å, b=11.867(2) Å, c = 12.676(3) Å, and Z = 4. Least-squares refinement of the structure led to a R(wR2) factor of 0.0251 (0.0621) for 2203 unique reflections of I>2σ(I) and for 306 variables. Ⅲ crystallizes in the monoclinic system, space group P21/n with cell parameters a=11.399(3) Å, b=14.718(4) Å, c=17.558(5) Å, β=97.79(2)°, and Z=4. Least-squares refinement of the structure led to a R(wR2) factor of 0.0571 (0.1384) for 3739 unique reflections of I>2σ(I) and for 344 variables. Structural studies showed that the relative orientations of the two phosphines in both complexes are different, probably due to the differences in the coordinating abilities between PMe3 and P(OMe)3 to the 5-coordinate fluxional intermediate.
Page
891 - 896
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