U3Yb2H26(C3O4)10 crystallizes in the triclinic P-1 space group. There are two inequivalent U sites. In the first U site, U(1) is bonded in a distorted pentagonal bipyramidal geometry to one O(1), one O(11), one O(12), one O(2), one O(4), one O(5), and one O(8) atom. The U(1)-O(1) bond length is 1.82 Å. The U(1)-O(11) bond length is 2.36 Å. The U(1)-O(12) bond length is 2.40 Å. The U(1)-O(2) bond length is 1.81 Å. The U(1)-O(4) bond length is 2.45 Å. The U(1)-O(5) bond length is 2.41 Å. The U(1)-O(8) bond length is 2.36 Å. In the second U site, U(2) is bonded in a distorted linear geometry to two equivalent O(14), two equivalent O(15), two equivalent O(3), and two equivalent O(7) atoms. Both U(2)-O(14) bond lengths are 2.54 Å. Both U(2)-O(15) bond lengths are 2.49 Å. Both U(2)-O(3) bond lengths are 1.82 Å. Both U(2)-O(7) bond lengths are 2.41 Å. Yb(1) is bonded in a 8-coordinate geometry to one O(10), one O(16), one O(17), one O(18), one O(19), one O(20), one O(6), and one O(9) atom. The Yb(1)-O(10) bond length is 2.29 Å. The Yb(1)-O(16) bond length is 2.31 Å. The Yb(1)-O(17) bond length is 2.30 Å. The Yb(1)-O(18) bond length is 2.37 Å. The Yb(1)-O(19) bond length is 2.32 Å. The Yb(1)-O(20) bond length is 2.34 Å. The Yb(1)-O(6) bond length is 2.33 Å. The Yb(1)-O(9) bond length is 2.30 Å. There are fifteen inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(10), one C(2), and one C(6) atom. The C(1)-C(10) bond length is 1.48 Å. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(6) bond length is 1.41 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-H(1) bond length is 1.09 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(11), one C(2), and one C(4) atom. The C(3)-C(11) bond length is 1.49 Å. The C(3)-C(4) bond length is 1.41 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(12), one C(3), and one C(5) atom. The C(4)-C(12) bond length is 1.50 Å. The C(4)-C(5) bond length is 1.40 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 H(2) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-H(2) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(1), one C(13), and one C(5) atom. The C(6)-C(13) bond length is 1.51 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(8), one C(9), and one H(3) atom. The C(7)-C(8) bond length is 1.40 Å. The C(7)-C(9) bond length is 1.40 Å. The C(7)-H(3) bond length is 1.09 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(15), one C(7), and one C(9) atom. The C(8)-C(15) bond length is 1.49 Å. The C(8)-C(9) bond length is 1.41 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(14), one C(7), and one C(8) atom. The C(9)-C(14) bond length is 1.51 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(4), and one O(5) atom. The C(10)-O(4) bond length is 1.28 Å. The C(10)-O(5) bond length is 1.28 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(10), and one O(11) atom. The C(11)-O(10) bond length is 1.25 Å. The C(11)-O(11) bond length is 1.30 Å. In the twelfth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(8), and one O(9) atom. The C(12)-O(8) bond length is 1.28 Å. The C(12)-O(9) bond length is 1.26 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(6), and one O(7) atom. The C(13)-O(6) bond length is 1.26 Å. The C(13)-O(7) bond length is 1.28 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(12), and one O(13) atom. The C(14)-O(12) bond length is 1.28 Å. The C(14)-O(13) bond length is 1.26 Å. In the fifteenth C site, C(15) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(14), and one O(15) atom. The C(15)-O(14) bond length is 1.27 Å. The C(15)-O(15) bond length is 1.28 Å. There are thirteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a distorted linear geometry to one O(13) and one O(16) atom. The H(4)-O(13) bond length is 1.66 Å. The H(4)-O(16) bond length is 1.00 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(16) atom. The H(5)-O(16) bond length is 0.98 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(17) atom. The H(6)-O(17) bond length is 0.99 Å. In the seventh H site, H(7) is bonded in a single-bond geometry to one O(17) atom. The H(7)-O(17) bond length is 1.00 Å. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(18) atom. The H(8)-O(18) bond length is 0.98 Å. In the ninth H site, H(9) is bonded in a single-bond geometry to one O(18) atom. The H(9)-O(18) bond length is 0.99 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one O(19) atom. The H(10)-O(19) bond length is 0.99 Å. In the eleventh H site, H(11) is bonded in a single-bond geometry to one O(19) atom. The H(11)-O(19) bond length is 0.99 Å. In the twelfth H site, H(12) is bonded in a single-bond geometry to one O(20) atom. The H(12)-O(20) bond length is 0.97 Å. In the thirteenth H site, H(13) is bonded in a distorted single-bond geometry to one O(11) and one O(20) atom. The H(13)-O(11) bond length is 1.69 Å. The H(13)-O(20) bond length is 0.99 Å. There are twenty inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to one U(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one U(1) atom. In the third O site, O(3) is bonded in a single-bond geometry to one U(2) atom. In the fourth O site, O(4) is bonded in an L-shaped geometry to one U(1) and one C(10) atom. In the fifth O site, O(5) is bonded in a distorted L-shaped geometry to one U(1) and one C(10) atom. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(13) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one U(2) and one C(13) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one U(1) and one C(12) atom. In the ninth O site, O(9) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(12) atom. In the tenth O site, O(10) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(11) atom. In the eleventh O site, O(11) is bonded in a distorted trigonal planar geometry to one U(1), one C(11), and one H(13) atom. In the twelfth O site, O(12) is bonded in a distorted single-bond geometry to one U(1) and one C(14) atom. In the thirteenth O site, O(13) is bonded in a distorted single-bond geometry to one C(14) and one H(4) atom. In the fourteenth O site, O(14) is bonded in a distorted single-bond geometry to one U(2) and one C(15) atom. In the fifteenth O site, O(15) is bonded in a distorted single-bond geometry to one U(2) and one C(15) atom. In the sixteenth O site, O(16) is bonded in a distorted trigonal non-coplanar geometry to one Yb(1), one H(4), and one H(5) atom. In the seventeenth O site, O(17) is bonded in a distorted water-like geometry to one Yb(1), one H(6), and one H(7) atom. In the eighteenth O site, O(18) is bonded in a distorted water-like geometry to one Yb(1), one H(8), and one H(9) atom. In the nineteenth O site, O(19) is bonded in a distorted water-like geometry to one Yb(1), one H(10), and one H(11) atom. In the twentieth O site, O(20) is bonded in a distorted water-like geometry to one Yb(1), one H(12), and one H(13) atom. Linkers: 3 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O. Metal clusters: 2 [Yb] ,3 [U]. The MOF has largest included sphere 4.68 A, density 2.60 g/cm3, surface area 2131.51 m2/g, accessible volume 0.10 cm3/g