The binuclear complex tris(ethylenediamine)zinc tetracyanozincate was prepared and characterized by single-crystal X-ray structure analysis. It consists of distorted [Zn(en)(3)](2+) octahedra and [Zn(CN)(4)](2-) tetrahedra. The thermolysis under air was studied by thermogravimetry, and the resulting product (ZnO) was characterized by X-ray diffraction and scanning electron microscopy, showing compact particles with a diameter of 100-300 nm. (c) 2006 Elsevier B.V. All rights reserved.