Rb2C6H3(NO3)3 crystallizes in the triclinic P-1 space group. There are two inequivalent Rb sites. In the first Rb site, Rb(1) is bonded in a 10-coordinate geometry to one O(1), one O(3), one O(4), one O(5), one O(6), one O(9), two equivalent O(2), and two equivalent O(7) atoms. The Rb(1)-O(1) bond length is 3.08 Å. The Rb(1)-O(3) bond length is 2.79 Å. The Rb(1)-O(4) bond length is 3.18 Å. The Rb(1)-O(5) bond length is 3.19 Å. The Rb(1)-O(6) bond length is 2.79 Å. The Rb(1)-O(9) bond length is 3.05 Å. There is one shorter (3.13 Å) and one longer (3.26 Å) Rb(1)-O(2) bond length. There is one shorter (2.96 Å) and one longer (3.07 Å) Rb(1)-O(7) bond length. In the second Rb site, Rb(2) is bonded in a 8-coordinate geometry to one O(1), one O(2), one O(3), one O(4), one O(5), one O(9), and two equivalent O(8) atoms. The Rb(2)-O(1) bond length is 2.99 Å. The Rb(2)-O(2) bond length is 3.24 Å. The Rb(2)-O(3) bond length is 2.83 Å. The Rb(2)-O(4) bond length is 2.97 Å. The Rb(2)-O(5) bond length is 3.13 Å. The Rb(2)-O(9) bond length is 2.86 Å. There is one shorter (2.87 Å) and one longer (3.15 Å) Rb(2)-O(8) bond length. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one N(1) atom. The C(1)-C(2) bond length is 1.47 Å. The C(1)-C(6) bond length is 1.38 Å. The C(1)-N(1) 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), one C(3), and one O(3) atom. The C(2)-C(3) bond length is 1.44 Å. The C(2)-O(3) bond length is 1.26 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(4), and one N(2) atom. The C(3)-C(4) bond length is 1.44 Å. The C(3)-N(2) bond length is 1.43 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one O(6) atom. The C(4)-C(5) bond length is 1.47 Å. The C(4)-O(6) bond length is 1.26 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4), one C(6), and one N(3) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-N(3) bond length is 1.42 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(1) atom. The C(6)-H(1) bond length is 1.09 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one C(1), one O(1), and one O(2) atom. The N(1)-O(1) bond length is 1.26 Å. The N(1)-O(2) bond length is 1.25 Å. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(3), one O(4), and one O(5) atom. The N(2)-O(4) bond length is 1.25 Å. The N(2)-O(5) bond length is 1.26 Å. In the third N site, N(3) is bonded in a trigonal planar geometry to one C(5), one O(7), and one O(8) atom. The N(3)-O(7) bond length is 1.26 Å. The N(3)-O(8) bond length is 1.27 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(6) atom. In the second H site, H(2) is bonded in a single-bond geometry to one O(9) atom. The H(2)-O(9) bond length is 0.98 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(9) atom. The H(3)-O(9) bond length is 0.99 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Rb(1), one Rb(2), and one N(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one Rb(2), two equivalent Rb(1), and one N(1) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Rb(1), one Rb(2), and one C(2) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one Rb(1), one Rb(2), and one N(2) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one Rb(1), one Rb(2), and one N(2) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Rb(1) and one C(4) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to two equivalent Rb(1) and one N(3) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to two equivalent Rb(2) and one N(3) atom. In the ninth O site, O(9) is bonded in a water-like geometry to one Rb(1), one Rb(2), one H(2), and one H(3) atom. Linkers: 2 O=C1[C]([N+](=O)[O-])C=C([N+](=O)[O-])C(=O)[C]1[N+](=O)[O-]. Metal clusters: 4 [Rb]. The MOF has largest included sphere 1.58 A, density 2.47 g/cm3, surface area 2693.05 m2/g, accessible volume 0.04 cm3/g