Synthesis and Crystal Structure of Bis(diphenylphosphino)methane Dipalladium(I) Complex with 2-Vinylpyridine (vpy). [Pd_2(μ-dppm)_2(vpy)Cl]ClO_4

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The bis(diphenylphosphino)methane dipalladium(I) complex: with 2-vinylpyridine, [Pd_2(μ-dppm)_2(vpy)Cl]ClO_4 (1) has been prepared and characterized crystallographically. Two Pd atoms are doubly bridged by two dppm ligands to form an eight-membered Pd_2P_4C_2 ring framework in a twist-chair conformation. Each Pd atoms are also coordinated by Cl^- ion and N atom of vpy ligand to provide a side-by-side conformation. The Pd-Pd distance of 2.597(2)Å is rather shorter than that (2.75Å) in the Pd metal, indicative of the existence of a direct Pd-Pd bond. On the eight-membered Pd_2C_2P_4 ring, the torsion angle of 43.2° is close to 45° and the Pd-Pd bond of 2.597(2)Å is also shorter than those in other dipalladium(I) dppm complexes. It has been experimentally found that the closer torsion angle is to 45°, the shorter Pd-Pd distance is. Complex 1 has the following crystal data: orthorhombic, P2_12_12_1, a=11.882(5), 6=11.909(7), c=38.676(5)Å, F=5473(3)Å^3, Z=4, R=0.048 and R_w=0.046.
近畿大学の論文
1997-03-05