Ni3C20H8(N3O2)4 crystallizes in the triclinic P-1 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a rectangular see-saw-like geometry to one N(1), one N(2), one N(5), and one O(1) atom. The Ni(1)-N(1) bond length is 2.09 Å. The Ni(1)-N(2) bond length is 2.06 Å. The Ni(1)-N(5) bond length is 2.13 Å. The Ni(1)-O(1) bond length is 2.04 Å. In the second Ni site, Ni(2) is bonded in an octahedral geometry to two equivalent N(6), two equivalent O(2), and two equivalent O(3) atoms. Both Ni(2)-N(6) bond lengths are 2.15 Å. Both Ni(2)-O(2) bond lengths are 2.03 Å. Both Ni(2)-O(3) bond lengths are 2.02 Å. There are ten 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 N(4) atom. The C(1)-C(2) bond length is 1.47 Å. The C(1)-N(1) bond length is 1.33 Å. The C(1)-N(4) bond length is 1.33 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one C(5), and one N(5) atom. The C(2)-C(5) bond length is 1.38 Å. The C(2)-N(5) bond length is 1.34 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(4), one N(5), and one H(1) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-N(5) bond length is 1.33 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(3), one N(6), and one H(2) atom. The C(4)-N(6) bond length is 1.33 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(2), one N(6), and one H(3) atom. The C(5)-N(6) bond length is 1.34 Å. The C(5)-H(3) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(1), and one O(2) atom. The C(6)-C(7) bond length is 1.51 Å. The C(6)-O(1) bond length is 1.26 Å. The C(6)-O(2) bond length is 1.26 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(10), one C(6), and one C(8) atom. The C(7)-C(10) bond length is 1.39 Å. The C(7)-C(8) bond length is 1.41 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(10), one C(7), and one C(9) atom. The C(8)-C(10) bond length is 1.39 Å. The C(8)-C(9) bond length is 1.51 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(3), and one O(4) atom. The C(9)-O(3) bond length is 1.26 Å. The C(9)-O(4) bond length is 1.22 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(7), one C(8), and one H(4) atom. The C(10)-H(4) bond length is 0.93 Å. There are six 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(2) atom. The N(1)-N(2) bond length is 1.34 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(1), one N(1), and one N(3) atom. The N(2)-N(3) bond length is 1.32 Å. In the third N site, N(3) is bonded in a water-like geometry to one N(2) and one N(4) atom. The N(3)-N(4) bond length is 1.34 Å. In the fourth N site, N(4) is bonded in a distorted single-bond geometry to one C(1) and one N(3) atom. In the fifth N site, N(5) is bonded in a trigonal planar geometry to one Ni(1), one C(2), and one C(3) atom. In the sixth N site, N(6) is bonded in a trigonal planar geometry to one Ni(2), one C(4), and one C(5) atom. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(10) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(6) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(6) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(9) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(9) atom. Linkers: 2 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O ,2 c1cnc(C2=NN=N[N]2)cn1. Metal clusters: 3 [Ni]. The MOF has largest included sphere 4.50 A, density 1.51 g/cm3, surface area 3459.53 m2/g, accessible volume 0.24 cm3/g