Issue 24, 2015

Pd-complex driven formation of single-chain nanoparticles


We report the facile synthesis of well-defined palladium(II) cross-linked single-chain nanoparticles (Pd-SCNPs) using the ‘repeating unit approach’. The linear precursor polymer (Mn ≈ 10 200 g mol−1, Đ ≈ 1.17) was synthesized via nitroxide mediated statistical copolymerization of styrene and 4-(chloromethyl)styrene (CMS) followed by a post-polymerization modification of the resulting copolymer to covalently attach the triarylphosphine ligand moieties. The ligand content along the lateral polymer chain was 12%. Intramolecular crosslinking was performed in diluted solution with a suitable precursor complex (Pd[1,5-cyclooctadiene]Cl2) to afford the well-defined Pd-SCNPs, which feature a hydrodynamic diameter of Dh = 5.4 nm. The palladium(II) containing single-chain nanoparticles were characterized in-depth using 1H NMR spectroscopy, 31P{1H} NMR spectroscopy, dynamic light scattering (DLS), size exclusion chromatography (SEC), 1H spin–spin relaxation time (T2) analysis, X-ray photoelectron spectroscopy (XPS), and log-normal distribution (LND) simulations. Finally, the applicability of the Pd-SCNPs as catalyst in the Sonogashira coupling was exemplified.

Graphical abstract: Pd-complex driven formation of single-chain nanoparticles

Supplementary files

Article information

Article type
18 Mar 2015
22 Apr 2015
First published
23 Apr 2015
This article is Open Access
Creative Commons BY license

Polym. Chem., 2015,6, 4358-4365

Author version available

Pd-complex driven formation of single-chain nanoparticles

J. Willenbacher, O. Altintas, V. Trouillet, N. Knöfel, M. J. Monteiro, P. W. Roesky and C. Barner-Kowollik, Polym. Chem., 2015, 6, 4358 DOI: 10.1039/C5PY00389J

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