Universität zu Köln

Tobechukwu Anthony, Eric ORCID: 0000-0002-0217-7585, Olthof, Selina, Roitsch, Stefan ORCID: 0000-0002-7233-2245, Meerholz, Klaus, Mathur, Sanjay ORCID: 0000-0003-2765-2693 and Klein, Axel ORCID: 0000-0003-0093-9619 (2025). A Bis‐Thiosemicarbazone Pd(II) SiO 2 Nanoparticle Conjugate for C─C Coupling Catalysis. European Journal of Inorganic Chemistry, 28 (23). pp. 1-12. Wiley. ISSN 1434-1948

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Abstract

[Artikel-Nr.: e202500245] Pd(II) complexes of thiosemicarbazones (TSCs) have previously been used as homogenous precatalysts for constructing C─C bonds. Herein, the first SiO2-supported homogeneous Pd(II)-TSC catalyst [PdL]–APTES–SiO 2 (APTES = (3-aminopropyl)triethoxysilane) is reported for this purpose. This Pd complex–SiO 2 nanoparticle (NP) conjugate is synthesized through covalent binding of the pentadentate bis(N4-(2-ethylphenyl)) 2,6-diacetyl-pyridine TSC onto monodispersed SiO 2 , followed by coordination of Pd(II). Characteristic shifts of resonances in the Fourier- transform infrared spectra allowed confirming the SiO 2 functionalization and the Pd-binding. High-resolution X-ray photoelectron spectroscopy (XPS) analysis of N 1s, C 1s, and S 2p shows that the binding energies of the atoms in the C═N, C═S, C─N, N─H, pyridine-N, and imine-N groups shift to lower values upon Pd coordination. The absence of chloride in the XPS of the H 2 L–APTES–SiO 2 conjugate strongly supports the successful covalent binding of the TSC onto the SiO 2 NPs and is in line with the S thiolate ^N imine ^N pyridine ^N amide coordina- tion of Pd(II) in the conjugate that is also found in the model complex [Pd(L)]. The [PdL]–APTES–SiO 2 NPs are used as precatalyst in Suzuki–Miyaura-type cross-coupling reactions with yields ranging from 70% to 83%

Item Type:	Article
Creators:	Creators Email ORCID ORCID Put Code Tobechukwu Anthony, Eric UNSPECIFIED https://orcid.org/0000-0002-0217-7585 UNSPECIFIED Olthof, Selina UNSPECIFIED UNSPECIFIED UNSPECIFIED Roitsch, Stefan UNSPECIFIED https://orcid.org/0000-0002-7233-2245 UNSPECIFIED Meerholz, Klaus UNSPECIFIED UNSPECIFIED UNSPECIFIED Mathur, Sanjay UNSPECIFIED https://orcid.org/0000-0003-2765-2693 UNSPECIFIED Klein, Axel UNSPECIFIED https://orcid.org/0000-0003-0093-9619 UNSPECIFIED
URN:	urn:nbn:de:hbz:38-803662
Identification Number:	10.1002/ejic.202500245
Journal or Publication Title:	European Journal of Inorganic Chemistry
Volume:	28
Number:	23
Page Range:	pp. 1-12
Number of Pages:	12
Date:	26 August 2025
Publisher:	Wiley
ISSN:	1434-1948
Language:	English
Faculty:	Faculty of Mathematics and Natural Sciences
Divisions:	Faculty of Mathematics and Natural Sciences > Department of Chemistry > Institute of Biochemistry
Subjects:	Chemistry and allied sciences Life sciences
Uncontrolled Keywords:	Keywords Language covalent functionalization ; palladium ; silica nanoparticles ; Suzuki–Miyaura cross-coupling ; thiosemicarbazones English
['eprint_fieldname_oa_funders' not defined]:	Publikationsfonds UzK
Refereed:	Yes
URI:	http://kups.ub.uni-koeln.de/id/eprint/80366