Synthesis and X-ray crystal structure of the chloride-bridged pace-sharingbioctahedral dirhodium complex [HP-i-Pr-3][Rh2Cl7(P-i-Pr-3)(2)]

The reaction of an ethanolic suspension of [NH4](3)[RhCl6] and P-i-Pr-3, in the presence of concentrated HCl, for 24h, gives [HP-i-Pr-3][Rh2Cl7(P-i-Pr -3)(2)], 1, in 18.5% yeild and a small amount of Rh(H)(Cl)(2)(P-i-Pr-3)(2), 2, The dinuclear complex 1 was characterized by elemental analyses, IR, H- 1, P-31 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. Cry stallographic data for 1 (at 298 K) are a = 15.944(3), b = 22.413(4), c = 1 1.500(4)Angstrom, space group Pna2(1) (Z = 4).