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In the search for soluble and reactive ruthenium nitrosyl complexes, [Ru(NO)('py bu S 4 ')]Br ([2]Br) was synthesized by template alkylation of NBu 4 [Ru(NO)(' bu S 2 ') 2 ] with py(CH 2 ,Br) 2  ['py bu S 4 ' 2- = 2,6-bis(2-mercapto-3,5-di-tert-butyl-phenylthio)dimethylpyridine(2-); ' bu S 2 ' 2-  = 2-mercapto-3,5-di-tert-butylphenylthiolate(2-); py(CH 2 Br) 2  = 2,6-bis(bromomethyl)pyridine]. The solid state structure of 2 has been determined by X-ray diffraction, which reveals a head-to-head O-O interaction between the linear Ru-NO entities. The ligand CH 2  protons of [2] +  are activated and exchange with D +  under ambient conditions. The ν (NO) band of [2]Br appears at 1841 cm -1  in the solid state (KBr or hostaflon mull) and is significantly blue-shifted in solution (1879 cm -1  in MeOH, 1886 cm -1  in DMF). A similar blue-shift (1866 cm -1  in KBr vs. 1888 cm -1  in MeOH) has been found for [Ru(NO)('pyS 4 ')]Br ([1]Br) which contains the parent [Ru(NO)('pyS 4 ')] +  cation ['pyS 4 ' 2- = 2,6-bis(2-mercaptophenylthio)dimethylpyridine(2-)]. These ν(NO) shifts can be explained either by an interionic charge-transfer between the bromide anions and the nitrosyl complex cation or by O-O interactions between two NO ligands as found for solid-state [2]Br. These interactions are not found for [1]OTs which exhibits a ν(NO) band at ca. 1890 cm -1  in the solid state (KBr, hostaflon) as well as in MeOH solution.

zeitschrift für naturforschung b

Übergangsmetallkomplexe mit Schwefelliganden, 145 [1]. [Ru(NO)('py bu S 4 ')]Br, ein Komplex mit [Ru(NO)(NS 4 )]-Gerüst, aktivierten CH 2 -Gruppen und interionischen Wechselwirkungen im Festkörper ['py bu S 4 ' 2-  = 2,6-Bis(2-mercapto-3,5-di-terM&gt;utylphenylthio) dimethylpyridin(2-)] /  Transition Metal Complexes with Sulfur Ligands, 145 [1]. [Ru(NO)('py bu S 4  ')]Br, a Complex with [Ru(NO)(NS 4 )] Core, Activated CH 2  Groups, and Interionic Interactions in the Solid State ('py bu S 4 ' 2-  = 2,6-Bis(2-mercapto-3,5-di-terf-butylphenylthio)dimethylpyridine(2-))