SYNTHESIS AND X-RAY CRYSTAL STRUCTURE OF THE CHLORIDE-BRIDGED FACE-SHARING BIOCTAHEDRAL DIRHODIUM COMPLEX [HP-i-Pr3][Rh2Cl7(P-i-Pr3)2

Abstract

The reaction of an ethanolic suspension of [NH4]3RhCl6] and P-i′-Pr3, in the presence of concentrated HC1, for 24h, gives [HP-i-Pr3][Rh2Cl7(P-i-Pr3)2], 1, in 18.5% yeild and a small amount of Rh(H)(Cl)2(P-i-Pr3)2, 2. The dinuclear complex 1 was characterized by elemental analyses, IR, 1H, 31P NMR spectroscopy, and single crystal X-ray analysis. However, when the above reaction is continued for 48 h one obtains only 2, in good yield. It is proposed that complex 1 is a reaction intermediate leading to 2. Crystallographic data for 1 (at 298 K) are a = 15.944(3), b = 22.413(4), c= 11.500(4) Å, space group Pna2x (Z = 4).