UP2H8(CO)6 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 4-coordinate geometry to one O(2), one O(4), one O(8), and one O(9) atom. The U(1)-O(2) bond length is 2.39 Å. The U(1)-O(4) bond length is 2.32 Å. The U(1)-O(8) bond length is 2.32 Å. The U(1)-O(9) bond length is 2.33 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(5) atoms. Both U(2)-O(1) bond lengths are 2.29 Å. Both U(2)-O(5) bond lengths are 2.31 Å. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(6) bond length is 1.40 Å. The C(1)-C(7) bond length is 1.51 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 H(1) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-H(1) bond length is 0.95 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-C(8) bond length is 1.51 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 H(2) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-H(2) bond length is 0.95 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(9) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-C(9) bond length is 1.51 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(3) atom. The C(6)-H(3) bond length is 0.95 Å. In the seventh C site, C(7) is bonded in a distorted water-like geometry to one C(1); one P(1); and two equivalent H(4,5) atoms. The C(7)-P(1) bond length is 1.79 Å. Both C(7)-H(4,5) bond lengths are 0.99 Å. In the eighth C site, C(8) is bonded in a distorted water-like geometry to one C(3); one P(2); and two equivalent H(6,7) atoms. The C(8)-P(2) bond length is 1.79 Å. Both C(8)-H(6,7) bond lengths are 0.99 Å. In the ninth C site, C(9) is bonded in a distorted water-like geometry to one C(5); one P(3); and two equivalent H(8,9) atoms. The C(9)-P(3) bond length is 1.79 Å. Both C(9)-H(8,9) bond lengths are 0.99 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded in a tetrahedral geometry to one C(7), one O(1), one O(2), and one O(3) atom. The P(1)-O(1) bond length is 1.52 Å. The P(1)-O(2) bond length is 1.51 Å. The P(1)-O(3) bond length is 1.57 Å. In the second P site, P(2) is bonded in a tetrahedral geometry to one C(8), one O(4), one O(5), and one O(6) atom. The P(2)-O(4) bond length is 1.50 Å. The P(2)-O(5) bond length is 1.53 Å. The P(2)-O(6) bond length is 1.56 Å. In the third P site, P(3) is bonded in a tetrahedral geometry to one C(9), one O(7), one O(8), and one O(9) atom. The P(3)-O(7) bond length is 1.57 Å. The P(3)-O(8) bond length is 1.50 Å. The P(3)-O(9) bond length is 1.51 Å. There are nine 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(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4,5) is bonded in a single-bond geometry to one C(7) atom. In the fifth H site, H(6,7) is bonded in a single-bond geometry to one C(8) atom. In the sixth H site, H(8,9) is bonded in a single-bond geometry to one C(9) atom. In the seventh H site, H(10) is bonded in a single-bond geometry to one O(3) atom. The H(10)-O(3) bond length is 0.94 Å. In the eighth H site, H(11) is bonded in a single-bond geometry to one O(6) atom. The H(11)-O(6) bond length is 0.94 Å. In the ninth H site, H(12) is bonded in a single-bond geometry to one O(7) atom. The H(12)-O(7) bond length is 0.94 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one U(2) and one P(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one U(1) and one P(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one P(1) and one H(10) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one U(1) and one P(2) atom. In the fifth O site, O(5) is bonded in a 2-coordinate geometry to one U(2) and one P(2) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one P(2) and one H(11) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one P(3) and one H(12) atom. In the eighth O site, O(8) is bonded in a distorted linear geometry to one U(1) and one P(3) atom. In the ninth O site, O(9) is bonded in a distorted bent 150 degrees geometry to one U(1) and one P(3) atom. Linkers: 2 [O]P(=O)(O)Cc1cc(CP([O])(=O)O)cc(CP([O])(=O)O)c1. Metal clusters: 3 [U]. The MOF has largest included sphere 4.99 A, density 1.90 g/cm3, surface area 2630.91 m2/g, accessible volume 0.27 cm3/g