The synthesis and X-ray crystal structure of a new molecular clip 2 was reported. It （C24H24N4O2, Mr = 400.47） crystallizes in the space group C2/c with a = 15.587（2）, b = 8.5805（12）, c = 15.259（2） A, β = 102.448（3）°, V= 1992.9 （5）A63, Z = 4, Dc = 1.335 g/cm63,μ = 0.087 mm^-1 and F（000） = 848. It remains monomeric in the crystal and a tape-like structure is formed in the crystal structure of molecular clip. The most unusual structural feature of 2 is the boat conformation of its cyclohexyl ring imposed by the ring fusion at C（9）-C（9a）.
The synthesis and X-ray crystal structure of a methylene-bridged glycoluril dimer 2 was reported.The methylene-bridged glycoluril dimer 2（C38H36Br4N8O12,Mr=1116.35） crystallizes in space group P1 with a=10.5802（6）,b=16.8469（9）,c=24.7673（14） ,α=98.00,β=96.263（1）,γ=101.606（1）o,V=4239.3（4）3,Z=4,Dc=1.749 g/cm3,μ=3.869 mm-1 and F（000）=2224.It crystallizes in an S-shaped conformation that displays two ethoxycarbonyl groups on each face of the molecule.
A new macrocycle based on diethoxycarbonyl glycoluril 3,C26H30N6O10,has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 12.7291（10）,b = 25.157（2）,c = 8.5489（7） A,β = 104.4760（10）°,V = 2650.7（4） A^3,Z = 4,C26H30N6O10,Mr = 586.56,F（000） = 1232,T = 292（2） K,Dc = 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 architecture is formed via intermolecular hydrogen bonding interactions.
