The reaction of (η5-C5H5)Mo(μ-I)(I)(NO)2] with the Hg derivatives of substituted N,N-dimethylbenzylamines [Hg(Q dmba)2] (HQ = substituted N,N-dimethylbenzylamine affords the organomolybdenum complexes [(η5-C5H5Mo(Qdmba)(I)(NO)] (2a-2e) in nearly quantitative yield as a racemic mixture of both enantiomers. When the reaction is carried out with HgS-C6H4C(H)(Me)NMe2)2, a 1 : 1 mixture of both diastereoisomers [(η5-C5H5)MoS-C6H4C(H)(Me)NMe2-2(I)(NO)] (2f-2g) is obtained. The resolution of this mixture can be accomplished by fractional crystallization in CH2Cl2/hexane. The X-ray crystal structure of the complexes (SPY-5-15-A, C)-[η5-C5H5)MoC6H2-(OCH2O)-2,3-CH2NMe2-6(I)(NO)] (2b) and (SPY-5-15-C)-[(η5-C5H5)MoS-C6H4C(H)(Me)NMe2-2(I)(NO)](2f) are reported. © 1995.
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