NiCuH8(C3N2)4 crystallizes in the tetragonal P4_32_12 space group. Ni(1) is bonded in a T-shaped geometry to one N(5) and two equivalent N(3) atoms. The Ni(1)-N(5) bond length is 2.30 Å. Both Ni(1)-N(3) bond lengths are 2.08 Å. Cu(1) is bonded in a T-shaped geometry to one N(4) and two equivalent N(1) atoms. The Cu(1)-N(4) bond length is 2.03 Å. Both Cu(1)-N(1) bond lengths are 2.02 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(1) atom. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(1) bond length is 0.95 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(2) atom. The C(2)-N(3) bond length is 1.36 Å. The C(2)-H(2) bond length is 0.95 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(4), one N(3), and one H(3) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-N(3) bond length is 1.33 Å. The C(3)-H(3) bond length is 0.95 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3), one N(1), and one N(2) atom. The C(4)-N(1) bond length is 1.34 Å. The C(4)-N(2) bond length is 1.37 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(6), one N(2), and one N(4) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-N(2) bond length is 1.40 Å. The C(5)-N(4) bond length is 1.34 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(5), one N(5), and one H(4) atom. The C(6)-N(5) bond length is 1.33 Å. The C(6)-H(4) bond length is 0.95 Å. There are five inequivalent N sites. In the first N site, N(4) is bonded in a trigonal planar geometry to one Cu(1) and two equivalent C(5) atoms. In the second N site, N(5) is bonded in a trigonal planar geometry to one Ni(1) and two equivalent C(6) atoms. In the third 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 fourth N site, N(2) is bonded in a bent 120 degrees geometry to one C(4) and one C(5) atom. In the fifth N site, N(3) 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. Linkers: 4 c1ncc(nc1)[N]C1=[N]=C(C=N[CH]1)[N]c1nccnc1. Metal clusters: 4 [Cu] ,4 [Ni]. The MOF has largest included sphere 6.09 A, density 0.76 g/cm3, surface area 3893.66 m2/g, accessible volume 0.96 cm3/g