Synthesis and X-ray crystal structure of the chloride-bridged face-sharing bioctahedral dirhodium complex [HP-i-Pr_3][Rh_2Cl_7(P-i-Pr_3)_2]

摘要

The reaction of an ethanolic suspension of[NH_4]_3[RhCl_6] and P-I-Pr_3, in the presence of concentratedHCl, for 24h, gives [HP-i-Pr_3]_2], 1, in 18.5percent yield and asmall amount of Rh(H)(Cl)_2(P-i-Pr_3)_2, 2. The dinuclearcomplex 1 was characterized by elemental analyses, IR, ~(1)H,~(31)P NMR spectroscopy, and single crystal X-ray analysis.However, when the above reaction is continued for 48h oneobtains only 2, in good yield. It is proposed that complex 1 is areaction in intermediate leading to 2. Crystallographic data for 1(at 298K) are a=15.944(3), b=22.413(4), c=11.500(4) A, space group Pna2_1 (Z=4).