The reactions of imidazoquinoxaline and 1,3,5-H3 btc acid under different condition have been investigated. The different degree of hydrolysis reaction leads to two different adducts being produced, namely, [（Hdiam Quin）＋（H2btc）-]（1）, and [（diam Quin）4（Imi Quin）·4H2O]（2）. Both compounds were characterized by X-ray crystallography. Crystal data for 1： monoclinic, space group Pn with a = 9.868（2）, b = 5.3172（11）, c = 15.387（3）A, β = 91.10（3）°, C17H14N4O6, Mr = 370.32, V = 807.2（3）A3, Z = 2, Dc = 1.524 g/cm3, μ（Mo Kα） = 0.118 mm-1, F（000） = 384, the final R = 0.0385 and w R = 0.0869 for 2294 observed reflections（I 〉 2σ（I））. Crystal data for 2： triclinic, space group P1 with a = 9.825（2）, b = 14.144（3）, c = 16.054（3） A, α = 101.06（3）, β = 102.55（3）, γ = 92.46（3）°, C（44）H40N（20）O4, Mr = 912.96, V = 2128.8（7） A3, Z = 2, Dc = 1.424 g/cm3, μ（Mo Kα） = 0.099 mm-1, F（000） = 952, the final R = 0.0554 and w R = 0.1662 for 6563 observed reflections（I 〉 2σ（I））. X-ray diffraction analysis reveals that compound 1 is a salt. Imidazoquinoxaline was wholly hydrolyzed into 2,3-diaminoquinoxaline and protonated as a cation with H2btc-acting as an anion. However, in compound 2, the imidazoquinoxaline is only partly hydrolyzed, and the resulting 2,3-diaminoquinoxaline forms adduct with the intacted imidazoquinoxaline. Both are further aggregated into 3D frameworks by strong hydrogen bonding even π-π interactions.
