The title compound has been synthesized by alkylation of diphenylglycoluril with o-xylylenedihalides followed by Sonogashira cross-coupling reaction. The yielded product 2 was investigated with X-ray crystallographic, NMR, EI-MS, and IR techniques. The crystal belongs to a triclinic system, space group P-1 with unit cell parameters a = 10.5057(8) Å, b = 12.6915(9) Å, c = 13.3426(10) Å, α = 83.8540(10)o, β = 87.9360(10)o, γ = 75.5700(10)o, V = 1712.9(2) Å3, Z = 2, D
c
= 1.322, M
r
= 681.59, μ = 0.232 mm−1, F(000) = 708, R
1
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