Ni3C6N9H6O crystallizes in the cubic Fd-3c space group. Ni(1) is bonded in a square co-planar geometry to one N(2), two equivalent N(1), and one O(1) atom. The Ni(1)-N(2) bond length is 2.03 Å. Both Ni(1)-N(1) bond lengths are 2.03 Å. The Ni(1)-O(1) bond length is 2.04 Å. C(1) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(1) atom. The C(1)-N(1) bond length is 1.32 Å. The C(1)-N(2) bond length is 1.34 Å. The C(1)-H(1) bond length is 0.93 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a 3-coordinate geometry to one Ni(1), one C(1), and one N(1) atom. The N(1)-N(1) bond length is 1.36 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(1) and two equivalent C(1) atoms. H(1) is bonded in a single-bond geometry to one C(1) atom. O(1) is bonded in a trigonal planar geometry to three equivalent Ni(1) atoms. Linkers: 10 C1=NC=N[N]1 ,8 C1=NN=C[N]1 ,6 [N]1=CN=NC=1. Metal clusters: 8 N1=N[Ni]2=NN=[Ni](N=N[Ni]1)O2. The MOF has largest included sphere 7.89 A, density 1.31 g/cm3, surface area 3034.52 m2/g, accessible volume 0.42 cm3/g