Synthesis and Characterization of Cyclopentadienyl Sulfur Niobium Complexes
Authors
Gómez Rubio, Manuel; Hernández Prieto, Cristina; Martín Alonso, Avelino; Mena Montoro, Miguel; Santamaría Angulo, CristinaIdentifiers
Permanent link (URI): http://hdl.handle.net/10017/38634DOI: 10.1016/j.jorganchem.2019.06.022
ISSN: 0022-328X
Date
2019-10-01Embargo end date
2021-06-19Funders
Ministerio de Ciencia, Innovación y Universidades.
Universidad de Alcalá.
Bibliographic citation
Journal of Organometallic Chemistry, 2019, v. 897, p. 148-154
Keywords
Sulfur complexes
cyclopentadienyl ligand
niobium
metathesis reactions
Project
PGC2018-094007-B-I00
CCG2018/EXP-026
Document type
info:eu-repo/semantics/article
Version
info:eu-repo/semantics/publishedVersion
Rights
Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0)
© 2019 Elsevier
Access rights
info:eu-repo/semantics/openAccess
Abstract
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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