MnCl 2 · 4H 2O, Cu(NO 3) 2 · 3H 2O, tris(2-aminoethyl)amine (tren) and NH 4NCS in a 1:4:4:10 molar ratio in aqueous solution results a bimetallic compound of the type [Cu(tren)(NCS)] 4[Mn(NCS) 6] ( 1) which has been characterized by microanalytical, physicochemical, spectroscopic and magnetic results. The structure of the complex is determined by X-ray diffraction study. Some pertinent crystal data are: monoclinic, space group P21/ c, a = 11.0442(9) Å, b = 14.4923(12) Å, c = 19.2505(16) Å, β = 91.95(10)°, and Z = 4. The crystal structure consists of a hydrogen bonded 3D network of [Cu(tren)(NCS)] + and [Mn(NCS) 6] 4− ions. Manganese(II) has an MnN 6 chromophore bound by six N atoms of the terminal thiocyanates. Each copper(II) centre is five coordinated by one N atom of terminal thiocyanate and four N atoms of the tripod ligand. Four copper(II) units are hydrogen bonded to form a hydrogen bonded tetramer. Each manganese(II) in turn is further engaged in hydrogen bonding to four such tetramers leading to the 3D network. Variable-temperature magnetic study shows no significant magnetic interactions among the metal ions connected by hydrogen bonding.