Abstract: | A novel two‐dimensional 3d–4f heterometallic inorganic compound with the formula CuII3GdIII(μ3‐OH)6(μ3‐SH)(SO4)(H2O)3] ( 1 ) was synthesized by treating gadolinium nitrate, copper chloride and DTSA under hydrothermal conditions. The structure was determined by X‐ray crystallography. The crystal is of orthorhombic, space group P212121 with a = 6.63090(1) Å, b = 11.3145(3) Å, c = 15.7869(3) Å, Cu3GdH13O13S2, M = 633.09, Z =4, V = 1184.42(4) Å3, F(000) = 1200, R1 = 0.0244 and ωR = 0.0522. The solid‐state dc magnetic susceptibility measurements revealed antiferromagnetic interactions between the paramagnetic metal center ions. |