U3Zn2P8H8(CO6)4 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 7-coordinate geometry to one O(3), one O(4), one O(5), one O(6), one O(7), one O(8), and one O(9) atom. The U(1)-O(3) bond length is 2.34 Å. The U(1)-O(4) bond length is 2.43 Å. The U(1)-O(5) bond length is 2.34 Å. The U(1)-O(6) bond length is 2.25 Å. The U(1)-O(7) bond length is 2.23 Å. The U(1)-O(8) bond length is 2.30 Å. The U(1)-O(9) bond length is 2.62 Å. In the second U site, U(2) is bonded in a square co-planar geometry to two equivalent O(1) and two equivalent O(2) atoms. Both U(2)-O(1) bond lengths are 2.24 Å. Both U(2)-O(2) bond lengths are 2.30 Å. Zn(1) is bonded to one O(10), one O(11), one O(4), and one O(9) atom to form ZnO4 tetrahedra that share corners with two equivalent P(3)CO3 tetrahedra and corners with two equivalent P(4)CO3 tetrahedra. The Zn(1)-O(10) bond length is 1.92 Å. The Zn(1)-O(11) bond length is 1.91 Å. The Zn(1)-O(4) bond length is 1.99 Å. The Zn(1)-O(9) bond length is 2.01 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted tetrahedral geometry to one P(1); one P(4); and two equivalent H(1,2) atoms. The C(1)-P(1) bond length is 1.85 Å. The C(1)-P(4) bond length is 1.80 Å. Both C(1)-H(1,2) bond lengths are 0.97 Å. In the second C site, C(2) is bonded in a distorted tetrahedral geometry to one P(2), one P(3), one H(3), and one H(4) atom. The C(2)-P(2) bond length is 1.78 Å. The C(2)-P(3) bond length is 1.83 Å. The C(2)-H(3) bond length is 0.97 Å. The C(2)-H(4) bond length is 0.97 Å. There are four inequivalent P sites. In the first P site, P(1) is bonded to one C(1), one O(3), one O(5), and one O(7) atom to form distorted corner-sharing PCO3 tetrahedra. The P(1)-O(3) bond length is 1.52 Å. The P(1)-O(5) bond length is 1.50 Å. The P(1)-O(7) bond length is 1.51 Å. In the second P site, P(2) is bonded to one C(2), one O(1), one O(2), and one O(8) atom to form corner-sharing PCO3 tetrahedra. The P(2)-O(1) bond length is 1.54 Å. The P(2)-O(2) bond length is 1.53 Å. The P(2)-O(8) bond length is 1.49 Å. In the third P site, P(3) is bonded to one C(2), one O(11), one O(4), and one O(6) atom to form PCO3 tetrahedra that share  a cornercorner with one P(2)CO3 tetrahedra and corners with two equivalent Zn(1)O4 tetrahedra. The P(3)-O(11) bond length is 1.50 Å. The P(3)-O(4) bond length is 1.56 Å. The P(3)-O(6) bond length is 1.51 Å. In the fourth P site, P(4) is bonded to one C(1), one O(10), one O(12), and one O(9) atom to form PCO3 tetrahedra that share  a cornercorner with one P(1)CO3 tetrahedra and corners with two equivalent Zn(1)O4 tetrahedra. The P(4)-O(10) bond length is 1.50 Å. The P(4)-O(12) bond length is 1.63 Å. The P(4)-O(9) bond length is 1.50 Å. There are three inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(3) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(4) is bonded in a single-bond geometry to one C(2) atom. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one U(2) and one P(2) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one U(2) and one P(2) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one U(1) and one P(1) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one U(1), one Zn(1), and one P(3) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one U(1) and one P(1) atom. In the sixth O site, O(6) is bonded in a bent 150 degrees geometry to one U(1) and one P(3) atom. In the seventh O site, O(7) is bonded in a bent 150 degrees geometry to one U(1) and one P(1) atom. In the eighth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one U(1) and one P(2) atom. In the ninth O site, O(9) is bonded in a distorted bent 120 degrees geometry to one U(1), one Zn(1), and one P(4) atom. In the tenth O site, O(10) is bonded in a bent 150 degrees geometry to one Zn(1) and one P(4) atom. In the eleventh O site, O(11) is bonded in a bent 150 degrees geometry to one Zn(1) and one P(3) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to one P(4) atom. Linkers: 4 [O]P([O])(=O)CP([O])([O])=O. Metal clusters: 3 [U] ,2 [Zn]. The MOF has largest included sphere 5.00 A, density 2.88 g/cm3, surface area 1841.13 m2/g, accessible volume 0.12 cm3/g