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The synthesis of Au144(SR)60 nanoclusters is documented in a previous work and modified here (31). All the reactions were conducted at room temperature under ambient air. Typically, HAuCl4·4H2O (0.607 mmol, 250 mg) and TOABr (0.696 mmol, 380 mg) were added to a 100-ml single-neck round-bottom flask and mixed with 30 ml of methanol. After being vigorously stirred for 30 min, the solution color changed from yellow to dark red. Then, various thiols (3.19 mmol for each synthesis) were added to the solution at room temperature. A milky, white floc was generated immediately. After ~15 min, a fresh NaBH4 solution (6 mmol, 227 mg, dissolved in 10 ml of nanopure water) was rapidly added to the solution under vigorous stirring. The color of the solution immediately turned black and produced Au particles, which were precipitated out of the methanol solution. The reaction was stopped after ~4.5 hours, and then the solution was removed. Black precipitates were washed with excess methanol and collected by centrifugation. This wash/precipitation procedure was repeated several times. The crude products that were dissolved in 1 ml of CH2Cl2 were pipetted onto eight pieces of a PTLC plate (10 cm by 20 cm), and the separation was conducted in a developing tank (solvent: DCM/petroleum ether = 20:20, v/v) for ~5 min. Then, the band of Au144(SCH2Ph)60 in the PTLC plate was cut, and the nanoparticles were extracted with pure DCM and then dried by rotary evaporation. The yield of Au144(SCH2Ph)60 was 16% (on an Au atom basis). After trying various solutions and precipitants, it was determined that single crystals of Au144(SCH2Ph)60 could be acquired by vapor diffusion of acetonitrile into a toluene solution of Au144(SCH2Ph)60 over 1 week at room temperature. The synthesis and crystal growth of other thiolated Au144 compounds were conducted in the same manner.

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