Although the composition of the newly formed NC could not be identified, the single peak observed in the RP-HPLC (Figure ) and ESI-MS data (Figure ) prompted an attempt to crystallize the obtained NC. A rod-shaped single crystal was eventually grown from a mixture of dichloromethane and ethanol (Figure ) after multiple attempts using various crystallization methods and solvent combinations. SCXRD analysis revealed that the chemical composition of the new NC was [Au24Pt(TBBT)12(TDT)3] 0 (Table ), which agreed with the peak positions and isotopic pattern of the ESI-MS spectrum (Figure ).