Rb2UC16H4(N2O9)2 crystallizes in the triclinic P-1 space group. Rb(1) is bonded in a 8-coordinate geometry to one O(1), one O(3), one O(5), one O(7), two equivalent O(2), and two equivalent O(4) atoms. The Rb(1)-O(1) bond length is 2.91 Å. The Rb(1)-O(3) bond length is 2.91 Å. The Rb(1)-O(5) bond length is 3.49 Å. The Rb(1)-O(7) bond length is 2.95 Å. There is one shorter (2.84 Å) and one longer (3.22 Å) Rb(1)-O(2) bond length. There is one shorter (2.94 Å) and one longer (3.23 Å) Rb(1)-O(4) bond length. U(1) is bonded in a distorted linear geometry to two equivalent O(1) and two equivalent O(9) atoms. Both U(1)-O(1) bond lengths are 2.41 Å. Both U(1)-O(9) bond lengths are 1.81 Å. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(4), one C(5), and one N(1) atom. The C(1)-C(4) bond length is 1.41 Å. The C(1)-C(5) bond length is 1.51 Å. The C(1)-N(1) bond length is 1.34 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(3), one C(6), and one N(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-C(6) bond length is 1.50 Å. The C(2)-N(1) bond length is 1.33 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(7), and one N(2) atom. The C(3)-C(7) bond length is 1.50 Å. The C(3)-N(2) bond length is 1.34 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(1), one C(8), and one N(2) atom. The C(4)-C(8) bond length is 1.51 Å. The C(4)-N(2) bond length is 1.34 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(5)-O(1) bond length is 1.28 Å. The C(5)-O(2) bond length is 1.24 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(3), and one O(4) atom. The C(6)-O(3) bond length is 1.28 Å. The C(6)-O(4) bond length is 1.25 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(5), and one O(6) atom. The C(7)-O(5) bond length is 1.24 Å. The C(7)-O(6) bond length is 1.31 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(7), and one O(8) atom. The C(8)-O(7) bond length is 1.22 Å. The C(8)-O(8) bond length is 1.34 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a bent 120 degrees geometry to one C(1) and one C(2) atom. In the second N site, N(2) is bonded in a bent 120 degrees geometry to one C(3) and one C(4) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a linear geometry to one O(5) and one O(6) atom. The H(1)-O(5) bond length is 1.52 Å. The H(1)-O(6) bond length is 1.04 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(8) atom. The H(2)-O(8) bond length is 0.98 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one Rb(1), one U(1), and one C(5) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to two equivalent Rb(1) and one C(5) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Rb(1) and one C(6) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to two equivalent Rb(1) and one C(6) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Rb(1), one C(7), and one H(1) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one C(7) and one H(1) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one Rb(1) and one C(8) atom. In the eighth O site, O(8) is bonded in a water-like geometry to one C(8) and one H(2) atom. In the ninth O site, O(9) is bonded in a single-bond geometry to one U(1) atom. Linkers: 2 [O]C(=O)c1nc(C([O])=O)c(C(=O)O)nc1C(=O)O. Metal clusters: 2 [Rb] ,1 [U]. The MOF has largest included sphere 3.12 A, density 2.41 g/cm3, surface area 2582.22 m2/g, accessible volume 0.09 cm3/g