Allylpalladium complexes of pyridylselenolates as precursors for palladium selenides
Complexes [Pd(μ-SeC5H4N-n)(η3-allyl)]2 (n=2, 4; allyl=C3H5, C4H7) have been synthesized by the reaction of Na(SeC5H4N-n) with [Pd(μ-Cl)(η3-allyl)]2 and characterized by microanalyses, NMR spectroscopy and X-ray structure. Thermolysis of [Pd(μ-SeC5H4N-n)(η3-C4H7)]2 in furnace or by AACVD yielded nano...
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Veröffentlicht in: | Inorganica Chimica Acta 2017-10, Vol.467, p.221-226 |
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Sprache: | eng |
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Zusammenfassung: | Complexes [Pd(μ-SeC5H4N-n)(η3-allyl)]2 (n=2, 4; allyl=C3H5, C4H7) have been synthesized by the reaction of Na(SeC5H4N-n) with [Pd(μ-Cl)(η3-allyl)]2 and characterized by microanalyses, NMR spectroscopy and X-ray structure. Thermolysis of [Pd(μ-SeC5H4N-n)(η3-C4H7)]2 in furnace or by AACVD yielded nanocrystals or thin film of Pd7Se4 whereas in oleylamine it gives Pd17Se15.
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•Allylpalladium complexes of 2-/4-pyridylselenolates have been synthesized.•Se bridges palladium centers, N atom of the ligand is free in binuclear structure.•Thermolysis of [Pd(μ-SeC5H4N-n)(η3-C4H7)]2 in furnace or by AACVD yielded Pd7Se4.•Thermolysis of [Pd(μ-SeC5H4N-2)(η3-C4H7)]2 in oleylamine gives Pd17Se15.
The complexes [Pd(μ-SeC5H4N-n)(η3-allyl)]2 (n=2, 4; allyl=C3H5, C4H7) have been synthesized in dichloromethane-methanol by the reaction of Na(SeC5H4N-n) with [Pd(μ-Cl)(η3-allyl)]2 in high yield. The structure of [Pd(μ-SeC5H4N-4)(η3-C4H7)]2 was established by single-crystal X-ray diffraction analysis. Thermolysis of [Pd(μ-SeC5H4N-n)(η3-C4H7)]2 in furnace or by Aerosol-Assisted Chemical Vapor Deposition technique, yielded nanocrystals or thin film of Pd7Se4 whereas in oleylamine it gives Pd17Se15. The SEM images of Pd7Se4 showed spherical shaped particles. |
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ISSN: | 0020-1693 1873-3255 |
DOI: | 10.1016/j.ica.2017.08.004 |