A series of luminescent bis-cyclometalated alkynylgold(III) complexes have been synthesized and characterized. Some of the complexes have been demonstrated to exhibit gelation properties driven by 蟺鈥撓€ stacking and hydrophobic鈥揾ydrophobic interactions. The gelation properties have been investigated in detail through variable-temperature UV鈥搗is absorption and emission studies, and the morphology of the gels has also been characterized by scanning electron microscopy and transmission electron microscopy.