Synthesis and characterization of asymmetric C,N-cyclometallated complexes of Mo(II). X-ray crystal structures of 5-C5H5)Mo(I)(NO)> and 5-C5H5)Mo(I)(NO)>

Article abstract of DOI:10.1016/0022-328X(95)05429-S

The reaction of <(η⁵-C5H5)Mo(μ-I)(I)(NO)>2> with Hg derivatives of substituted N,N-dimethylbenzylamines (HQ = substituted N,N-dimethylbenzylamine affords the organomolybdenum complexes <(η⁵-C5H5)Mo(Qdmba)(I)(NO)> (2a-2e) in nearly quantitative yield as a racemic mixture of both enantiomers.When the reaction is carried out with Hg2, a 1:1 mixture of both diastereoisomers <(η⁵-C5H5)Mo(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)Mo(I)(NO)> (2b) and (SPY-5-15-C)-<(η⁵-C5H5)Mo(I)(NO)> (2f) are reported.Keywords: Molybdenum; Cyclometallation; Nitrosyl; Asymmetry; Iodide; Transmetallation