Cu3C16H8(N3O)4 crystallizes in the tetragonal I-42d space group. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a tetrahedral geometry to two equivalent N(2) and two equivalent N(3) atoms. Both Cu(1)-N(2) bond lengths are 1.95 Å. Both Cu(1)-N(3) bond lengths are 1.98 Å. In the second Cu site, Cu(2) is bonded in a square co-planar geometry to four equivalent O(1) atoms. All Cu(2)-O(1) bond lengths are 1.94 Å. There are four inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(4) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(3) bond length is 1.40 Å. The C(1)-C(4) bond length is 1.43 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1) and one N(2) atom. The C(2)-N(2) bond length is 1.15 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(1) and one N(3) atom. The C(3)-N(3) bond length is 1.15 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(1), one N(1), and one O(1) atom. The C(4)-N(1) bond length is 1.33 Å. The C(4)-O(1) bond length is 1.26 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one C(4), one H(1), and one H(2) atom. The N(1)-H(1) bond length is 0.88 Å. The N(1)-H(2) bond length is 0.88 Å. In the second N site, N(2) is bonded in a linear geometry to one Cu(1) and one C(2) atom. In the third N site, N(3) is bonded in a linear geometry to one Cu(1) and one C(3) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(1) atom. O(1) is bonded in a bent 120 degrees geometry to one Cu(2) and one C(4) atom. Linkers: 16 N#C[C](C#N)C(N)=O. Metal clusters: 12 [Cu]. The MOF has largest included sphere 4.21 A, density 1.51 g/cm3, surface area 4060.46 m2/g, accessible volume 0.26 cm3/g