The fabrication of nanocrystals (NCs) composed of the cationic Au(I) complex was demonstrated, by the reprecipitation method in which colloidal solution of the NCs showed brilliant green phosphorescence with a quantum yield of 83% in n-hexane. Characterization of the prepared NCs was performed by transmission electron microscopy observation and elemental analysis with energy-dispersive-X-ray. spectroscopy. The obtained Au(I) NCs were particles of random shapes with a diameter of 200-400 nm. The selected-area diffraction and X-ray diffraction measurements showed the characteristic diffraction patterns attributable to the crystal structure of the bulk crystal of the Au(I) complex. A similar method was performed with a different counteranion, leading to a colloidal solution of the microcrystals (MCs) with brilliant yellow phosphorescence and a quantum yield of 26% in n-hexane. Luminescence deposition onto an indium tin oxide. (ITO)-coated glass substrate, resulting in characteristic luminescence patterns on the ITO substrates with relatively high photoluminescence quantum yields.