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In a single pot synthesis consecutive reaction of the tetradentate amine-thiole H 2 - ' S 2 N 2 H 2 ' 2 ('S 2 N 2 H 2 ' 2-  = 1,2-ethanediamino-N,N'-bis(2-benzenethiolato)(2-)). with [LiN(SiMe 3 ) 2 ] and benzyl chloride (BzCl) yields the amine-thioether 'Bz 2 S 2 N 2 H 2 ' which gives the tertiary amine-thioether 'Bz 2 S 2 N 2 Me 2 ' when reacted with further [LiN(SiMe 3 ) 2 ] and CH 3 I Removal of the benzyl groups with an excess of sodium and acidification with hydrochloric acid finally yield H 2 - ' S 2 N 2 Me 2 ' I ('S 2 N 2 Me 2 ' 2-  = 1,2-ethanediamino-N,N'-di- methyl-N,N'-bis(2-benzenethiolato)(2-)). 1 and 2 have been characterized by X-ray structure analysis. With [Ni(CH 3 COO) 2 ] · 4H 2 O,1 yields racemic [Ni('S 2 N 2 Me 2 ')] 3 in a diastereospecific reaction. Crystallization of 3 leads to spontaneous resolution of the racemate. By X-ray structure analysis of 3 the absolute configuration in the single crystal examined was determi­ned using Roger's μ-refinement (μ = 1.00(4)). Upon reaction with [RuCl 3 ·3H 2 O]. LiOMe and CO. I yields [Ru(CO) 2 ('S 2 N 2 Me 2 ')] 5. Spectroscopic data indicate that 5 and the parent complex [Ru(CO) 2 ('S 2 N 2 H 2 ')] differ with respect to their core structures. Influence of the amine methylation on structure and reactivity of complexes with [M('S 2 N 2 R 2 ')] cores, R = H. Me, is discussed.

zeitschrift für naturforschung b

Übergangsmetallkomplexe mit Schwefelliganden, CVIII + . Eine bequeme Synthese des tertiären Amin-thiolat-Liganden 'S 2 N 2 Me 2 ' 2- . Einfluß der Aminmethylierung auf die Koordinationschemie von Nickel- und Ruthenium-Komplexen mit [M('S 2 N 2 R 2 ')]-Geriisten (R = H, CH 3 ). ('S 2 N 2 Me 2 ' 2-  = 1,2-Ethandiamin-N,N'-dimethyl-N,N'-bis(2-benzolthiolat)(2-)) / Transition Metal Complexes with Sulfur Ligands, CVIII + . A Facile Synthesis of the Tertiary Amine-thiolato Ligand 'S 2 N 2 Me 2 ' 2- . Influence of the Aminomethylation on the Coordination Chemistry of Nickel and Ruthenium Complexes with [M('S 2 N 2 R 2 ')] Frameworks (R = H, CH 3 ). ('S 2 N 2 Me 2 ' 2-  = 1,2-Ethanediamino-N,N'-dimethyl-N,N'-bis(2-benzenethiolato)(2-))