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2O, with further vigorous stirring, resulting in a rapid change to a opaque brown solution. The composition of the massive clusters generated is monitored by extracting small samples on a time scale of a few minutes to several days; these are washed with ethanol, redissolved in toluene, and analyzed mass spectrometrically as described in the text. After 15 min the analysis of this particular preparation shows predominantly the 14 k compound, along with indications of much lighter unresolved material. After several hours the 22 k is predominant, and after 1 day the 28 k is also strongly observed.
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6 sample showed mass fractions for C (0.1126), H (0.0211), S (0.0515), and Au (0.8184). with impurities from other starting materials totaling to <0.02. Molar ratios found for S:C (5.84:1) and H:C (2.23:1) agree well with the 6:1 and 2.2:1 ratios calculated for the thiol(ate), whereas the 2.57:1 ratio for Au:S would indicate that a cluster of ∼145 atoms has a coverage of ∼56 thiol(ate) groups.
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