NiCuC8H4(NS)4(CH)2 crystallizes in the monoclinic P2/m space group. The structure consists of two acetylene molecules inside a NiCuC8H4(NS)4 framework. In the NiCuC8H4(NS)4 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a square co-planar geometry to two equivalent S(1) and two equivalent S(2) atoms. Both Ni(1)-S(1) bond lengths are 2.16 Å. Both Ni(1)-S(2) bond lengths are 2.16 Å. In the second Ni site, Ni(2) is bonded in a square co-planar geometry to four equivalent S(3) atoms. All Ni(2)-S(3) bond lengths are 2.16 Å. Cu(1) is bonded in a rectangular see-saw-like geometry to one N(1), one N(2), and two equivalent N(3) atoms. The Cu(1)-N(1) bond length is 2.04 Å. The Cu(1)-N(2) bond length is 2.04 Å. Both Cu(1)-N(3) bond lengths are 2.04 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one S(1) atom. The C(1)-C(2) bond length is 1.43 Å. The C(1)-N(1) bond length is 1.34 Å. The C(1)-S(1) bond length is 1.72 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one N(2), and one S(2) atom. The C(2)-N(2) bond length is 1.34 Å. The C(2)-S(2) bond length is 1.72 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(3), one N(3), and one S(3) atom. The C(3)-C(3) bond length is 1.43 Å. The C(3)-N(3) bond length is 1.34 Å. The C(3)-S(3) bond length is 1.72 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(5), one N(1), and one H(1) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-N(1) bond length is 1.35 Å. The C(4)-H(1) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4); one N(2); and one H(2,3) atom. The C(5)-N(2) bond length is 1.35 Å. The C(5)-H(2,3) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted trigonal planar geometry to one C(6); one N(3); and one H(2,3) atom. The C(6)-C(6) bond length is 1.38 Å. The C(6)-N(3) bond length is 1.35 Å. The C(6)-H(2,3) bond length is 1.09 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(4) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cu(1), one C(2), and one C(5) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Cu(1), one C(3), and one C(6) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2,3) is bonded in a single-bond geometry to one C(5) atom. There are three inequivalent S sites. In the first S site, S(1) is bonded in a water-like geometry to one Ni(1) and one C(1) atom. In the second S site, S(2) is bonded in a water-like geometry to one Ni(1) and one C(2) atom. In the third S site, S(3) is bonded in a water-like geometry to one Ni(2) and one C(3) atom. Linkers: 4 S=C1N=CC=NC1=S. Metal clusters: 2 [Cu] ,2 [Ni]. The MOF has largest included sphere 3.45 A, density 1.90 g/cm3, surface area 3373.62 m2/g, accessible volume 0.11 cm3/g