Inorganic Chemistry, Vol.34, No.7, 1788-1792, 1995
Protonation of Chloride in Os(H)(2)Cl-2(Pipr3)(2) - Synthesis of ((Pipr3)(2)H2Os(Mu-Cl)(3)Osh2(Pipr3)(2))Cf3So3
Protonation (CF3SO3H) of Os(H)(2)Cl(2)L(2) (L = (PPr3)-Pr-i) in Et(2)O or CH2Cl2 yields Os-2(H)(4)(mu-Cl)(3)L(4)(+), characterized by IR, H-1 NMR, and P-31 NMR spectroscopy elemental analysis, and X-ray diffraction. The reaction thus involves selectivity for protonation at chloride (vs H or Os) and eliminates HCl. The dimetal cation reacts with [NBu(4)]Cl to regenerate Os(H)(2)Cl(2)L(2). Crystal data (-169 degrees C) for [Os-2(H)(4)Cl-3((PPr3)-Pr-i)(4)]CF3SO3 . CH2Cl2 : a = 16.859(4) Angstrom, b = 18.719(5) Angstrom, c = 18.488(5) Angstrom, beta = 113.85(1)degrees with Z = 4 in space group P2(1)/a.