We have successfully synthesized single crystals of C60 fullerene complex with a symmetrical triplet donor of 2,3,6,7,10,11-hexamethoxytriphenylene (HMT). All spectroscopie data and analyses support the chemical composition of this complex as C60(HMT)2. Single crystals of C60(HMT)2 are, at 20±1 °C, cubic, space group Fd3c-O
8 (No. 228) with a = 30.251(9) Å, α = 90.00°, V = 27682(30) Å3, Z = 16 (dcalcd = 1.476 gcm-3), and R
(unweighted) = 0.098.