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  Synthesis of a Cu-Filled Rh17S15 Framework: Microwave Polyol Process Versus High-Temperature Route

Roslova, M., Golub, P., Opherden, L., Ovchinnikov, A., Uhlarz, M., Baranov, A. I., et al. (2017). Synthesis of a Cu-Filled Rh17S15 Framework: Microwave Polyol Process Versus High-Temperature Route. Inorganic Chemistry, 56(19), 11513-11523. doi:10.1021/acs.inorgchem.7b01102.

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Item Permalink: http://hdl.handle.net/11858/00-001M-0000-002E-133A-E Version Permalink: http://hdl.handle.net/21.11116/0000-0001-9CA6-4
Genre: Journal Article

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 Creators:
Roslova, Maria1, Author
Golub, Pavlo1, Author
Opherden, Lars1, Author
Ovchinnikov, Alexander2, Author              
Uhlarz, Marc1, Author
Baranov, Alexey I.2, Author              
Prots, Yurii1, Author
Isaeva, Anna1, Author
Coduri, Mauro1, Author
Herrmannsdörfer, Thomas1, Author
Wosnitza, Joachim1, Author
Doert, Thomas1, Author
Ruck, Michael3, Author              
Affiliations:
1External Organizations, ou_persistent22              
2Chemical Metal Science, Max Planck Institute for Chemical Physics of Solids, Max Planck Society, ou_1863405              
3Michael Ruck, Max Planck Fellow, Max Planck Institute for Chemical Physics of Solids, Max Planck Society, ou_1863444              

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 Abstract: Metal-rich, mixed copper rhodium sulfide Cu3-delta Rh34S30 that represents a new Cu-filled variant of the Rh17S15 structure has been synthesized and structurally characterized. Copper content in the [CuRh8] cubic cluster was found to vary notably dependent on the chosen synthetic route. Full site occupancy was achieved only in nanoscaled Cu3Rh34S30 obtained by a rapid, microwave-assisted reaction of CuCl, Rh-2(CH3CO2)(4) and thiosemicarbazide at 300 degrees C in just 30 min; whereas merely Cu-deficient Cu3-delta Rh34S30 (2.0 >= delta >= 0.9) compositions were realized via conventional high-temperature ceramic synthesis from the elements at 950 degrees C. Although Cu3-delta Rh34S30 is metallic just like Rh17S15, the slightly enhanced metal content has a dramatic effect on the electronic properties. Whereas the Rh17S15 host undergoes a superconducting transition at 5.4 K, no signs of the latter were found for the Cu-derivatives at least down to 1.8 K. This finding is corroborated by the strongly reduced density of states at the Fermi level of the ternary sulfide and the disruption of long-range Rh Rh interactions in favor of Cu-Rh interactions as revealed by quantum-chemical calculations.

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Language(s): eng - English
 Dates: 2017-09-132017-09-13
 Publication Status: Published in print
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Title: Inorganic Chemistry
  Abbreviation : Inorg. Chem.
Source Genre: Journal
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Publ. Info: Washington, DC : American Chemical Society
Pages: - Volume / Issue: 56 (19) Sequence Number: - Start / End Page: 11513 - 11523 Identifier: ISSN: 0020-1669
CoNE: /journals/resource/0020-1669