Synthesis and structural characterization of trithiocarbonate complexes of molybdenum and ruthenium derived from CS2 ligand
Résumé
In an effort to synthesize trithiocarbonate complexes of molybdenum and ruthenium, we carried out the reaction of CS2 with the intermediates, obtained from the reaction of [(CpML3X)-M-#], (1: Cp-# = C5Me5, M = Mo, L-1 = L-2 = L-3 = CO, X = Me; 2: Cp-# = C5H5, M = Ru, L-1 = L-2 = PPh3, X = Cl and 3: Cp-# = C5H5, M = Fe, L-1 = L-2 = CO, X = I) and [LiBH4 center dot thf]. The reactions led to formation of the trithiocarbonate complexes [Cp*Mo(CO)(2)(mu-eta(2):eta(1)-CS3)(CO)(3)MoCp*] (4) [Cp*Mo(CO)(2)(eta(2)-S2CSMe)] (5) and [Cp*Mo(-CO)(2)(eta(2)-S2CMe)] (6) in moderate yields. Treatment of [CpRu(PPh3)(2)Cl] (2) with [LiBH4 center dot thf] followed by mild pyrolysis of CS2 yielded the trithiocarbonate ruthenium complex [CpRuPPh3(eta(2)-S2CSMe)] (7). All the new compounds have been characterized by various spectroscopic techniques and the structures of compounds 4, 5 and 7 were unequivocally established by crystallographic analysis. (C) 2017 Published by Elsevier B.V.