NiCuC12H8(N2O)4 crystallizes in the monoclinic C2/c space group. Ni(1) is bonded to two equivalent N(1), two equivalent N(2), and two equivalent O(2) atoms to form NiN4O2 octahedra that share edges with two equivalent Cu(1)N2O4 octahedra. Both Ni(1)-N(1) bond lengths are 2.06 Å. Both Ni(1)-N(2) bond lengths are 2.10 Å. Both Ni(1)-O(2) bond lengths are 2.11 Å. Cu(1) is bonded to two equivalent N(2), two equivalent O(1), and two equivalent O(2) atoms to form distorted CuN2O4 octahedra that share edges with two equivalent Ni(1)N4O2 octahedra. Both Cu(1)-N(2) bond lengths are 2.01 Å. Both Cu(1)-O(1) bond lengths are 1.97 Å. Both Cu(1)-O(2) bond lengths are 2.57 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(4) bond length is 1.40 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one N(1), and one H(2) atom. The C(2)-N(1) bond length is 1.35 Å. The C(2)-H(2) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(6), one N(1), and one H(3) atom. The C(3)-C(6) bond length is 1.39 Å. The C(3)-N(1) bond length is 1.35 Å. The C(3)-H(3) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(1), one C(5), and one C(6) atom. The C(4)-C(5) bond length is 1.50 Å. The C(4)-C(6) bond length is 1.40 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(1), and one O(2) atom. The C(5)-O(1) bond length is 1.28 Å. The C(5)-O(2) bond length is 1.27 Å. In the sixth C site, C(6) is bonded in a distorted trigonal planar geometry to one C(3), one C(4), and one H(4) atom. The C(6)-H(4) bond length is 1.09 Å. There are four inequivalent N sites. In the first N site, N(3) is bonded in a linear geometry to one N(2) and one N(4) atom. The N(3)-N(2) bond length is 1.22 Å. The N(3)-N(4) bond length is 1.16 Å. In the second N site, N(4) is bonded in a single-bond geometry to one N(3) atom. In the third N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(1), one Cu(1), and one N(3) atom. In the fourth N site, N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(2), and one C(3) atom. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(5) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Ni(1), one Cu(1), and one C(5) atom. Linkers: 4 [O]C(=O)c1ccncc1. Metal clusters: 2 [Cu] ,2 [Ni]. The MOF has largest included sphere 3.06 A, density 1.76 g/cm3, surface area 3439.56 m2/g, accessible volume 0.13 cm3/g