RbLiC4H6O7 crystallizes in the monoclinic C2/c space group. There are two inequivalent Rb sites. In the first Rb site, Rb(1) is bonded in a 10-coordinate geometry to two equivalent O(4), two equivalent O(5), two equivalent O(6), and four equivalent O(3) atoms. Both Rb(1)-O(4) bond lengths are 3.05 Å. Both Rb(1)-O(5) bond lengths are 3.22 Å. Both Rb(1)-O(6) bond lengths are 3.23 Å. There are two shorter (2.97 Å) and two longer (3.20 Å) Rb(1)-O(3) bond lengths. In the second Rb site, Rb(2) is bonded in a 8-coordinate geometry to two equivalent H(3), two equivalent O(1), two equivalent O(5), and two equivalent O(6) atoms. Both Rb(2)-H(3) bond lengths are 3.07 Å. Both Rb(2)-O(1) bond lengths are 3.09 Å. Both Rb(2)-O(5) bond lengths are 2.88 Å. Both Rb(2)-O(6) bond lengths are 2.97 Å. Li(1) is bonded to one O(6), one O(7), and two equivalent O(2) atoms to form edge-sharing LiO4 tetrahedra. The Li(1)-O(6) bond length is 1.89 Å. The Li(1)-O(7) bond length is 1.91 Å. There is one shorter (1.95 Å) and one longer (1.96 Å) Li(1)-O(2) bond length. There are four inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(2) bond length is 1.27 Å. In the second C site, C(2) is bonded in a distorted water-like geometry to one H(5) and one O(3) atom. The C(2)-H(5) bond length is 1.11 Å. The C(2)-O(3) bond length is 1.42 Å. In the third C site, C(3) is bonded in a distorted water-like geometry to one H(6) and one O(4) atom. The C(3)-H(6) bond length is 1.10 Å. The C(3)-O(4) bond length is 1.42 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(5) and one O(6) atom. The C(4)-O(5) bond length is 1.27 Å. The C(4)-O(6) bond length is 1.27 Å. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(3) atom. The H(1)-O(3) bond length is 0.99 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(4) atom. The H(2)-O(4) bond length is 0.99 Å. In the third H site, H(3) is bonded in a distorted linear geometry to one Rb(2), one O(5), and one O(7) atom. The H(3)-O(5) bond length is 1.58 Å. The H(3)-O(7) bond length is 1.02 Å. In the fourth H site, H(4) is bonded in a distorted single-bond geometry to one O(7) atom. The H(4)-O(7) bond length is 1.00 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(2) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(3) atom. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a 1-coordinate geometry to one Rb(2) and one C(1) atom. In the second O site, O(2) is bonded in a distorted T-shaped geometry to two equivalent Li(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to two equivalent Rb(1), one C(2), and one H(1) atom. In the fourth O site, O(4) is bonded in a distorted water-like geometry to one Rb(1), one C(3), and one H(2) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Rb(1), one Rb(2), one C(4), and one H(3) atom. In the sixth O site, O(6) is bonded in a 2-coordinate geometry to one Rb(1), one Rb(2), one Li(1), and one C(4) atom. In the seventh O site, O(7) is bonded in a 3-coordinate geometry to one Li(1), one H(3), and one H(4) atom. Linkers: 2 [O]C(=O)[C@@H](O)[C@H](O)C([O])=O ,2 [O]C(=O)[C@H](O)[C@@H](O)C([O])=O ,4 O. Metal clusters: 4 [Rb] ,4 [Li]. The MOF has largest included sphere 1.96 A, density 2.20 g/cm3, surface area 2639.33 m2/g, accessible volume 0.05 cm3/g