In this paper, one imidazole macrocyclic divalent cation with flexible configuration was chosen with the aim of the immobilization of its conformation. One novel organic-inorganic hybrid supramolecule {[syn/anti-did] (CuS3C3N3) (C2H3N)} (1), [did2+ = (12z, 52z)–11H, 51H–1, 5(1, 3)-diimidazol-3-iuma-3, 7(1, 2)-dibenzenacyclooctaphane-13, 53-diium] has been synthesized through the self-assembly reaction of did2+ with CuSCN under solvothermal reaction. This compound has been unambiguously confirmed by PXRD, IR, TG and X-ray single crystal diffraction. Crystallographic analysis shows that the anion of compound 1 is binuclear structure. The stability of compound 1 is relatively good.