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Solid-state NMR and EXAFS spectroscopic characterization of polycrystalline copper(I) O,O '-dialkyldithiophosphate cluster compounds : formation of copper(I) O,O '-diisobutyldithiophosphate compounds on the surface of synthetic chalcocite
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Rusanova, Daniela, Pike, Kevin J., Persson, Ingmar, Hanna, John V., Dupree, Ray, Forsling, Willis and Antzutkin, Oleg N. (2006) Solid-state NMR and EXAFS spectroscopic characterization of polycrystalline copper(I) O,O '-dialkyldithiophosphate cluster compounds : formation of copper(I) O,O '-diisobutyldithiophosphate compounds on the surface of synthetic chalcocite. Chemistry: A European Journal, Volume 12 (Number 20). pp. 5282-5292. doi:10.1002/chem.200501490 ISSN 0947-6539.
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Official URL: http://dx.doi.org/10.1002/chem.200501490
Abstract
A number of polycrystalline copper(I) O,O'-dialkyldithiophosphate cluster compounds with Cu-4, Cu-6, and Cu-8 cores were synthesized and characterized by using extended X-ray absorption fine-structure (EXAFS) spectroscopy. The structural relationship of these compounds is discussed. The polycrystalline copper(i) O,O'-diisobutyldithiophosphate cluster compounds, [Cu-8{S2P(OiBu)(2),}(6)(S)] and [CU6{S2P(OiBU)(2)}(6)], were also characterized by using P-31 CP/MAS NMR (CP = cross polarization, MAS = magic-angle spinning) and static Cu-65 NMR spectroscopies (at different magnetic fields) and powder X-ray diffraction (XRD) analysis. Comparative analyses of the P-31 chemical-shift tensor, and the Cu-65 chemical shift and quadrupolar-splitting parameters, estimated from the experimental NMR spectra of the polycrystalline copper(I) cluster compounds, are presented. The adsorption mechanism of the potassium O,O'-diisobutyldithiophosphate collector, K[S2P(OiBu)(2)], at the surface of synthetic chalcocite (Cu2S) was studied by means of solid-state P-31 CP/MAS NMR spectroscopy and scanning electron microscopy (SEM). P-31 NMR resonance lines from collector-treated chalcocite surfaces were assigned to a mixture of [Cu-8{S2P(OiBu)(2)}(6)(S)] and [Cu-6- {S2P(OiBu)(2)}(6)] compounds.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry | ||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
Journal or Publication Title: | Chemistry: A European Journal | ||||
Publisher: | Wiley - V C H Verlag GmbH & Co. KGaA | ||||
ISSN: | 0947-6539 | ||||
Official Date: | 5 July 2006 | ||||
Dates: |
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Volume: | Volume 12 | ||||
Number: | Number 20 | ||||
Number of Pages: | 11 | ||||
Page Range: | pp. 5282-5292 | ||||
DOI: | 10.1002/chem.200501490 | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Access rights to Published version: | Restricted or Subscription Access |
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