Triclinic single crystals of Cu 4 (H 3 N-(CH 2 ) 9 -NH 3 )(OH) 2 [C 6 H 2 (COO) 4 ] 2 ·5H 2 O were prepared in aqueous solution at 80°C in the presence of 1,9-diaminononane. Space group P1 (no. 2) with a = 1057.5(2), b = 1166.0(2), c = 1576.7(2) pm, α = 106.080(10)°, β = 90.73(2)°and γ = 94.050(10)°. The four crystallographic independent Cu 2+ ions are surrounded by five oxygen atoms each with Cu-O distances between 191.4(3) and 231.7(4) pm. The connection between the Cu 2+ coordination polyhedra and the [C 6 H 2 (COO) 4 ] 4anions yields three-dimensional framework with negative excess charge and wide