Abstract
The reactions of [Cp 2MO 2(CO) 4] ( 1) with 2,2′-dipyridyl disulphide (C 5H 4NS) 2, 8,8′-diquinolyl disulphide (C 9H 6NS) 2 and tetramethyl thiuram disulphide (Me 2NC(S)S) 2 in toluene solution resulted in the cleavage of the MoMo triple bond to yield molybdenum complexes [CpMo(CO) 2(C 5H 4NS)] ( 2),[CpMo(CO) 2(C 9H 6NS)] ( 3) and [CpMo(CO) 2(S 2CNMe 2)] ( 4), respectively. The molecular structures of 2, 3 · OPPh 3 and 4 were determined by X-ray diffraction studies. Crystals of 2 are monoclinic, space group P2 1/ n, with Z = 4, in a unit cell of dimensions a = 6.448(1), b = 12.616(2), c = 14.772(2) Å β = 92.85(1)°. The structure was refined to R = 0.028 and R W = 0.039 for 1357 observed reflections. Crystals of 3 · OPPh 3 are triclinic, spacegroup P 1 , with Z = 2, in a unit cell of dimensions a = 11.351(3), b = 13.409(3), c = 9.895(2) Å α = 94.59(2), β = 90.35(2), γ = 78.07(2)°. The structure was refined to R = 0.033 and R w = 0.037 for 3260 observed reflections. Crystals of 4 are monoclinic, space group P2 1/ a and Z = 4 with a = 12.468(5), b = 7.637(2), c = 13.135(4) Å β = 96.62(3)°. The structure was refined to R = 0.032 and R W = 0.042 for 1698 observed reflections. Each of complexes 2– 4 contains a cyclopentadienyl ligand, a cis pair of carbonyls and a chelate ligand (S,N donor or S,S donor). All the compounds have distorted square-pyramid structures.
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