The reduction of hydrated ruthenium(III) chloride with zinc in the presence of cyclooctadiene: Molecular structure of Ru(C 8H 10)(C 8H 12) and isolation and x-ray structural characterization of Ru 2Cl 4(C 8H 12) 2, RuH(C 8H 11)(C 6H 6) and Ru 3Cl 3(OCH 3)(C 8H 12) 3

Abstract

The preparation of Ru(C 8H 10)(C 8H 12) ( 1) by reduction of hydrated ruthenium trichloride with zinc in the presence of cyclooctadiene occasionally results in mixtures from which the addition compound Ru 2Cl 4(C 8H 12) 2·RuH(C 8H 11)(C 6H 6)·0.5C 6H 6( 2· 3·0.5C 6H 6) and the trinuclear complex Ru 3Cl 3(OCH 3)(C 8H 12) 3 (4) could be isolated. Complexes 1–4 were characterized by X-ray crystallography. Relevant crystallographic data are: 1: orthorhombic Pna2 1, a = 2159.7(9), b = 878.9(4), c = 692.4(4) pm, Z = 4, R = 0.029, R w = 0.030 (2281 data). 2·3·0.5C 6H 6: triclinic P 1 , a = 773.8(2), b = 1316.9(2), c = 1766.9(6) pm, α = 72.40(2), β = 79.70(3), γ = 74.78(2)°, Z = 2, R = 0.051, R w = 0.061 (9564 data). 4: orthorhombic Pna2 1, a = 1784.6(4), b = 939.5(1), c = 3076.3(7) pm, Z = 8, R = 0.070, R w = 0.075 (2805 data).