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Transition Metal Complexes with Sulfur Ligands, XCl+ Fe(II) Complexes of the Pentadentate Thioether-Thiolate-Amine Ligand tBuNHS'-H2: Synthesis, Characterization, Reactivity and Stereochemistry (tBuNHS4'-H2 = 2,2'-Bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine)
Sellmann, Dieter,Soglowek, Wolfgang,Moll, Matthias
, p. 1105 - 1114 (2007/10/02)
In search of model compounds for the active centers of nitrogenases, tBuNHS4')> complexes of the pentadentate thioether-thiolate-amine ligand tBuNHS42- (tBuNHS4'-H2 = 2,2'-bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine) were obtained.Alkylation of tBuS2'-H2 with (BrC2H4)2NH yielded the new ligand tBuNHS4'-H2 as a mixture of positional isomers.Isolation of single isomers was achieved by reacting the mixture with FeCl2*4H2O and CO in order to give the corresponding complexes which were separated and hydrolyzed to yield the free ligands.Reaction of tBuNHS4'-H2 with FeCl2*4H2O led to the high-spin complex tBuNHS4')> which is extremely air-sensitive in solution.It rapidely reacts with L = CO, NO, PMe3, and N2H4, and is the most suitable starting material for syntheses of tBuNHS4')> complexes which were characterized for L = CO, NO+, NO, PMe3 and N2H4.All complexes are considerably better soluble in organic solvents than the corresponding parent compounds HS4')>, ('NHS4'-H2 = 2,2'-bis(2-mercaptophenylthio)diethylamine), but have similar properties in most other respects.In the oxidation of tBuNHS4')> at low temperatures, there is evidence for the formation of the diazene complex tBuNHS4')>2>. Iron Complexes, Thioether-Thiolate Ligand, Synthesis
