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Übergangsmetallkomplexe mit Schwefelliganden, 145 [1]. [Ru(NO)('pybuS4')]Br, ein Komplex mit [Ru(NO)(NS4)]-Gerüst, aktivierten CH2-Gruppen und interionischen Wechselwirkungen im Festkörper ['pybuS4'2- = 2,6-Bis(2-mercapto-3,5-di-terM>utylphenylthio) dimethylpyridin(2-)] / Transition Metal Complexes with Sulfur Ligands, 145 [1]. [Ru(NO)('pybuS4 ')]Br, a Complex with [Ru(NO)(NS4)] Core, Activated CH2 Groups, and Interionic Interactions in the Solid State ('pybuS4'2- = 2,6-Bis(2-mercapto-3,5-di-terf-butylphenylthio)dimethylpyridine(2-))
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Dieter Sellmann
,
Daniel Häußinger
Published/Copyright:
June 2, 2014
Abstract
In the search for soluble and reactive ruthenium nitrosyl complexes, [Ru(NO)('pybuS4')]Br ([2]Br) was synthesized by template alkylation of NBu4[Ru(NO)('buS2')2] with py(CH2,Br)2 ['pybuS4'2-= 2,6-bis(2-mercapto-3,5-di-tert-butyl-phenylthio)dimethylpyridine(2-); 'buS2'2- = 2-mercapto-3,5-di-tert-butylphenylthiolate(2-); py(CH2Br)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 CH2 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)('pyS4')]Br ([1]Br) which contains the parent [Ru(NO)('pyS4')]+ cation ['pyS4'2-= 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.
Received: 2000-4-5
Published Online: 2014-6-2
Published in Print: 2000-8-1
© 1946 – 2014: Verlag der Zeitschrift für Naturforschung
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Articles in the same Issue
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- Hydrogen Bonds in "Carboxyoximes": the Case of Bomane Derivatives
- Thermal Decomposition of Prussian Blue Analogues of the Type Fe[Fe(CN)5NO]
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