A series of conducting mixed-metallic coordination polymers: Cu 2 Pb(SCN) 4 , CuPb(SeCN) 4 , Cu II 0:50 Cu I Pb (SCN AE SeCN) 2 , CuAg(SCN) 2 , CuAg(SeCN) 2 and CuAg(SCN AE SeCN) have been synthesized by the reaction of Cu II and Pb II or Ag I nitrates with KSCN or KSeCN, or both KSCN and KSeCN in H 2 O. Of significance are the aerobic reactions which yield heterometallic complexes via oxidation of SCN ) and SeCN ) into (SCN) 2 and (SeCN) 2 followed by quantitative reduction of Cu II into Cu I ; in the case of CuPb(SeCN) 4 reduction of Cu II into Cu I is not observed, while in Cu II 0:50 Cu I Pb(SCN AE SeCN) 2 , Cu II is partially reduced to Cu I . These compounds have been characterized by elemental (C, N, S and Se) analyses, magnetic moment measurements, relevant spectroscopies (i.r., far i.r., Raman, u.v.-vis. and e.p.r.), powder X-ray diffraction pattern and conductivity technique. The v(CBN) vibrations in 2162-2087 cm )1 and far i.r. bands (500-100 cm )1 ) corroborated by Raman bands are conclusive of the bridging (N, S/Se) mode and metal-NCS and metal-SCN/SeCN ) bonding respectively in the complexes. Room temperature magnetic moment, electronic absorption spectra and e.p.r. active/silent nature confirm the oxidation state of copper in these solids. Room temperature compressed pellet conductivities r rt , 10 )9 to 10 )7 S cm )1 with activation energies, E a ¼ 0.19-0.25 eV and increase in the conductivity with increase in temperature in the 305-423 K, range and decrease in conductivity with decrease in temperature in the 295-200 K range, show their semiconductor properties.