Synthesis of cyclopentadienyl ruthenium complexes containing 5-membered N-heterocyclic thiolates
摘要:
Mononuclear ruthenium-thiolate complexes of structural type CpRu(PPh3)(2)SR (1) [R = 2-imidazolyl (a), 1-methylimidazolyl (b), 5-methyl-1,3,5-thiadiazolyl (c) and 5-methyl-4H-1,2,4-triazolyl (d)] are accessible from the reaction of CpRu(PPh3)(2)Cl with the corresponding thiolate anions. Reaction of CpRu(PPh3)(2)Cl with the heterocyclic-thiolate anions in the presence of the bisphosphine ligands affords CpRu(P-P) SR [P-P = bis(diphenylphosphino) methane; dppm (2), bis(diphenylphosphino) ethane; dppe (3)]. If CO gas was bubbled through a THF solution of 1b, the complex CpRu(PPh3)(CO)S(C4N2H5) (4b) is produced. These ruthenium-heterocyclic thiolate complexes have been characterized by elemental analysis, spectroscopy (IR, H-1, P-31{H-1} NMR and MS) and cyclic voltammetry for some samples. The solid-state structures of 3a and 3b are determined by single-crystal X-ray structure analysis. (C) 2010 Elsevier B.V. All rights reserved.