Synthesis and Characterization of (Tris(3,5-dimethylpyrazolyl)borato)rhodium Alkyl and Vinyl Chloride Complexes.

Abstract

A series of complexes of the type Tp'Rh(CNCH(2)CMe(3))(R)Cl, where R = CH(3), CD(3), n-propyl, isopropyl, cyclopropyl, and vinyl and Tp' = tris(3,5-dimethylpyrazolyl)borate have been synthesized and fully characterized. The complexes are prepared by reaction of the corresponding Grignard reagent with Tp'Rh(CNCH(2)CMe(3))Cl(2), which in turn is synthesized from Tp'Rh(NCCH(3))Cl(2). The complex Tp'Rh(CNCH(2)CMe(3))(isopropyl)Cl crystallizes in orthorhombic space group Pbcn (No. 60) with a = 27.8224(1) Å, b = 14.2541(2) Å, c = 14.5549(2) Å, Z = 8, and V = 5772.23(9) Å(3). The complex Tp'Rh(CNCH(2)CMe(3))(cyclopropyl)Cl crystallizes in monoclinic space group P2(1)/c (No. 14) with a = 9.573(2) Å, b = 18.933(3) Å, c = 17.873(14) Å, beta = 103.70(4) degrees, Z = 4, and V = 3147(3) Å(3). The complex Tp'Rh(PMe(3))Cl(2) crystallizes in monoclinic space group P2(1)/n (No. 14) with a = 10.9384(6) Å, b = 17.3111(9) Å, c = 13.5132(7) Å, beta = 111.536(1) degrees, Z = 4, and V = 2378.5(2) Å(3).