RbC2H2(N3O)2 crystallizes in the monoclinic P2_1/c space group. Rb(1) is bonded in a 9-coordinate geometry to one N(3), one N(4), one N(5), one N(6), two equivalent O(1), and three equivalent O(2) atoms. The Rb(1)-N(3) bond length is 3.19 Å. The Rb(1)-N(4) bond length is 3.15 Å. The Rb(1)-N(5) bond length is 3.17 Å. The Rb(1)-N(6) bond length is 3.03 Å. There is one shorter (3.18 Å) and one longer (3.34 Å) Rb(1)-O(1) bond length. There are a spread of Rb(1)-O(2) bond distances ranging from 2.87-3.06 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1), one N(3), and one N(4) atom. The C(1)-N(1) bond length is 1.37 Å. The C(1)-N(3) bond length is 1.34 Å. The C(1)-N(4) bond length is 1.35 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one N(5) atom. The C(2)-C(2) bond length is 1.44 Å. The C(2)-N(1) bond length is 1.39 Å. The C(2)-N(5) bond length is 1.32 Å. There are six inequivalent N sites. In the first N site, N(4) is bonded in a distorted trigonal planar geometry to one Rb(1), one C(1), one H(1), and one H(2) atom. The N(4)-H(1) bond length is 1.04 Å. The N(4)-H(2) bond length is 1.02 Å. In the second N site, N(5) is bonded in a distorted single-bond geometry to one Rb(1) and one C(2) atom. In the third N site, N(6) is bonded in a distorted trigonal non-coplanar geometry to one Rb(1), one N(1), and one N(2) atom. The N(6)-N(1) bond length is 1.39 Å. The N(6)-N(2) bond length is 1.34 Å. In the fourth N site, N(1) is bonded in a distorted water-like geometry to one C(1), one C(2), and one N(6) atom. In the fifth N site, N(2) is bonded in a distorted trigonal planar geometry to one N(6), one O(1), and one O(2) atom. The N(2)-O(1) bond length is 1.27 Å. The N(2)-O(2) bond length is 1.27 Å. In the sixth N site, N(3) is bonded in a distorted single-bond geometry to one Rb(1) and one C(1) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(4) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to two equivalent Rb(1) and one N(2) atom. In the second O site, O(2) is bonded in a 1-coordinate geometry to three equivalent Rb(1) and one N(2) atom. Linkers: 2 Nc1nnc(-c2nnc(N)n2[N][N+](=O)[O-])n1[N][N+](=O)[O-] ,2 Nc1nnc(-c2nn[c]n2[N][N+](=O)[O-])n1[N][N+](=O)[O-]. Metal clusters: 4 [Rb]. The MOF has largest included sphere 1.67 A, density 2.37 g/cm3, surface area 2894.04 m2/g, accessible volume 0.08 cm3/g