NiCuC8H4(NS)4 crystallizes in the tetragonal P4_2/mmc space group. Ni(1) is bonded in a square co-planar geometry to four equivalent S(1) atoms. All Ni(1)-S(1) bond lengths are 2.16 Å. Cu(1) is bonded in a rectangular see-saw-like geometry to four equivalent N(1) atoms. All Cu(1)-N(1) bond lengths are 2.05 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one N(1) and one S(1) atom. The C(1)-N(1) bond length is 1.34 Å. The C(1)-S(1) bond length is 1.71 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(1) atom. The C(2)-N(1) bond length is 1.35 Å. The C(2)-H(1) bond length is 1.09 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. H(1) is bonded in a single-bond geometry to one C(2) atom. S(1) is bonded in a water-like geometry to one Ni(1) and one C(1) atom. Linkers: 4 S=C1N=CC=NC1=S. Metal clusters: 2 [Cu] ,2 [Ni]. The MOF has largest included sphere 4.06 A, density 1.77 g/cm3, surface area 2989.29 m2/g, accessible volume 0.17 cm3/g