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Menard, Laurent D; Xu, Huiping; Gao, Shang-Peng; Twesten, Ray D; Harper, Amanda S; Song, Yang; Wang, Gangli; Douglas, Alicia D; Yang, Judith C; Frenkel, Anatoly I; Murray, Royce W; Nuzzo, Ralph G
The journal of physical chemistry. B, 08/2006, Volume: 110, Issue: 30Journal Article
The atomic metal core structures of the subnanometer clusters Au13PPh34S(CH2)11CH32Cl2 (1) and Au13PPh34S(CH2)11CH34 (2) were characterized using advanced methods of electron microscopy and X-ray absorption spectroscopy. The number of gold atoms in the cores of these two clusters was determined quantitatively using high-angle annular dark field scanning transmission electron microscopy. Multiple-scattering-path analyses of extended X-ray absorption fine structure (EXAFS) spectra suggest that the Au metal cores of each of these complexes adopt an icosahedral structure with a relaxation of the icosahedral strain. Data from microscopy and spectroscopy studies extended to larger thiolate-protected gold clusters showing a broader distribution in nanoparticle core sizes (183 ± 116 Au atoms) reveal a bulklike fcc structure. These results further support a model for the monolayer-protected clusters (MPCs) in which the thiolate ligands bond preferentially at 3-fold atomic sites on the nanoparticle surface, establishing an average composition for the MPC of Au180S(CH2)11CH340. Results from EXAFS measurements of a gold(I) dodecanethiolate polymer are presented that offer an alternative explanation for observations in previous reports that were interpreted as indicating Au MPC structures consisting of a Au core, Au2S shell, and thiolate monolayer.
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