The heteronuclear coordination polymer [Cd(SCN)(2)Ni(en)(NCS)(2)(EtOH)](2) 1 (en = ethylenediamine) was obtained by reaction of Cd(NO3)(2)center dot 4H(2)O, KSCN, Ni(NO3)(2)center dot 6H(2)O and en in a mote ration of 1:3:1:0.1 in ethanol solution. The complex is characterized by IR spectroscopy, electronic spectroscopy and single-crystal X-ray diffraction analysis. Crystal structure analyses show that the title complex belongs to the triclinic space group P (1) over bar with a=8.922(3), b=9.860(3), c=10.333(5) angstrom, alpha=113.116(6)degrees. beta=106.551)(6)degrees, gamma = 101.622(4)degrees. V = 749.0(5) angstrom(3). Cd(II) and Ni(II) centers are linked by di-mu-1,3-thiocyanate bridges to form a 2D network containing three types of 16-membered [Cd2Ni2(mu-1,3-SCN)(4)] macrocycles. Each Cd(II) center links six Ni(II) centers by six mu-1,3-SCN- bridges and each Ni(II) center links three Cd(II) centers by three mu-1,3-SCN- bridges. The luminescent properties of 1 in the solid state were investigated. (c) 2009 Elsevier B.V. All rights reserved.