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Authors
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Scharf, S.; Notz, S.; Pfefferkorn, K.; Rüffer, T.; Formánek, P.; Hübner, R.; Selyshchev, O.; Madeira, T. I.; Zahn, D. R. T.; Lang, H.
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Title
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Synthesis and twin polymerization of Si(OCH2py)4 for nitrogen-containing carbon materials
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Date
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12.01.2024
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Number
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0
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Abstract
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The synthesis and twin polymerization (TP) of Si(OCH2py)4 (3 a, py=2-cC5H4N; 3 b, py=3-cC5H4N; 3 c, py=4-cC5H4N) is discussed. The solid state structures of 3 b, c were confirmed by single-crystal X-ray crystallography showing non-conventional H-bonding, forming 2D chains (3 b) or 3D networks (3 c). Thermally induced TP of 3 a–c and their simultaneous polymerization with 2,2‘-spiro-bi[4H-1,3,2-benzodioxasiline] (4) is described. The resulting hybrid materials were characterized by 1H, 13C{1H}, and 29Si{1H} CP MAS NMR spectroscopy confirming the transformation of the SiOCH2 moieties into CH2 groups enabling the formation of the respective polymers. These results were supported by HAADF-STEM studies, displaying micro-structuring. Nitrogen-containing porous carbon materials C_1–C_3 show surface areas of 1300 and 1700 m2 g−1, large pore volumes between 0.6–1.2 cm3 g−1, and nitrogen contents of up to 3.1 at-%. X-ray photoemission spectroscopy reveal that pyrrolic, pyridine, and pyridone nitrogen atoms are present. If equimolar amounts of 3 a–c and 4 are simultaneously polymerized in the presence of [Pd(OAc)2] (5), then the Pd nanoparticle-decorated material Pd@C_3 (900 m2 g−1) was obtained, which showed k values of −0.083 and −0.066 min−1 in the reduction of methylene blue and methyl orange, proving the accessibility of the Pd NPs.
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Publisher
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Wiley
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Wikidata
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Citation
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European Journal of Inorganic Chemistry 27 (2024) e202300656
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DOI
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https://doi.org/10.1002/ejic.202300656
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Tags
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