Synthesis and characterization of cyclopentadienyl sulfur niobium complexes

Add time:08/02/2019    Source:sciencedirect.com

A trimetallic sulfide cluster [Nb3(η5-C5Me5)3Cl3(μ3-Cl)(μ-S)3(μ3-S)] (2) has been synthesized from the reaction of [Nb(η5-C5Me5)Cl4] (1) with (Me3Si)2S in a 4:3 ratio by the release of SiClMe3. The trinuclear nature of complex 2 has been established by single crystal X-ray diffraction analysis. Thermal treatment of 2 with SiH3Ph generated the dinuclear niobium(IV) complex [Nb2(η5-C5Me5)2Cl2(μ-S)2] (3) in a quantitative way. Likewise, one-pot syntheses of 3 has been developed from reaction of 1, (Me3Si)2S, and SiH3Ph in toluene. A series of dinuclear sulfide niobium(IV) derivatives [Nb2(η5-C5Me5)2R2(μ-S)2] (R = Me 4, Et 5, CH2SiMe3 6, C3H5 7, CH2Ph 8, nBu 9) can easily be obtained from the reaction of 3 with 2 equiv of the corresponding alkylating reagents. Single crystal X-ray diffraction analyses of 6 and 7 showed in all cases a trans disposition of the substituents.

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