A new macrocycle based on diethoxycarbonyl glycoluril 3, C_(26)H_(30)N_6O_(10), has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space groupP2_1/c with a= 12.7291(10),b = 25.157(2),c = 8.5489(7) (A),β= 104.4760(10)°, F=2650.7(4) (A)~3, Z = 4, C_(26)H_(30)N_6O_(10), M_r = 586.56, F(000) = 1232, T = 292(2) K, D_c = 1.470 g/cm~3,μ = 0.115 mm~(-1), the final R = 0.0590 and wR = 0.1299 for 4918 observed reflections with I > 2σ(I). In the structure of the title compound, a three-dimensional microporous ar...