U2C3P3NH10O9F crystallizes in the monoclinic C2/c 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(1), one O(2), one O(4), and one O(9) atom. The U(1)-O(1) bond length is 2.33 Å. The U(1)-O(2) bond length is 2.37 Å. The U(1)-O(4) bond length is 2.32 Å. The U(1)-O(9) bond length is 2.35 Å. In the second U site, U(2) is bonded in a pentagonal planar geometry to one O(5), one O(6), one O(7), and two equivalent F(1) atoms. The U(2)-O(5) bond length is 2.31 Å. The U(2)-O(6) bond length is 2.31 Å. The U(2)-O(7) bond length is 2.36 Å. There is one shorter (2.34 Å) and one longer (2.35 Å) U(2)-F(1) bond length. There are three inequivalent C sites. In the first C site, C(1) is bonded to one P(1), one N(1), one H(1), and one H(2) atom to form distorted corner-sharing CPH2N tetrahedra. The C(1)-P(1) bond length is 1.83 Å. The C(1)-N(1) bond length is 1.51 Å. The C(1)-H(1) bond length is 0.99 Å. The C(1)-H(2) bond length is 0.99 Å. In the second C site, C(2) is bonded to one P(2); one N(1); and two equivalent H(3,4) atoms to form distorted corner-sharing CPH2N tetrahedra. The C(2)-P(2) bond length is 1.83 Å. The C(2)-N(1) bond length is 1.51 Å. Both C(2)-H(3,4) bond lengths are 0.99 Å. In the third C site, C(3) is bonded to one P(3); one N(1); and two equivalent H(5,6) atoms to form distorted corner-sharing CPH2N tetrahedra. The C(3)-P(3) bond length is 1.81 Å. The C(3)-N(1) bond length is 1.50 Å. Both C(3)-H(5,6) bond lengths are 0.99 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded to one C(1), one O(1), one O(2), and one O(3) atom to form distorted PCO3 tetrahedra that share  a cornercorner with one N(1)HC3 tetrahedra. The P(1)-O(1) bond length is 1.51 Å. The P(1)-O(2) bond length is 1.53 Å. The P(1)-O(3) bond length is 1.51 Å. In the second P site, P(2) is bonded to one C(2), one O(4), one O(5), and one O(6) atom to form distorted PCO3 tetrahedra that share  a cornercorner with one N(1)HC3 tetrahedra. The P(2)-O(4) bond length is 1.51 Å. The P(2)-O(5) bond length is 1.53 Å. The P(2)-O(6) bond length is 1.50 Å. In the third P site, P(3) is bonded to one C(3), one O(7), one O(8), and one O(9) atom to form distorted PCO3 tetrahedra that share  a cornercorner with one N(1)HC3 tetrahedra. The P(3)-O(7) bond length is 1.49 Å. The P(3)-O(8) bond length is 1.56 Å. The P(3)-O(9) bond length is 1.49 Å. N(1) is bonded to one C(1), one C(2), one C(3), and one H(7) atom to form distorted NHC3 tetrahedra that share  a cornercorner with one P(1)CO3 tetrahedra,  a cornercorner with one P(2)CO3 tetrahedra, and  a cornercorner with one P(3)CO3 tetrahedra. The N(1)-H(7) bond length is 0.95 Å. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(1) atom. In the third H site, H(3,4) is bonded in a single-bond geometry to one C(2) atom. In the fourth H site, H(5,6) is bonded in a single-bond geometry to one C(3) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one N(1) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one O(3) atom. The H(8)-O(3) bond length is 0.96 Å. In the seventh H site, H(9) is bonded in a single-bond geometry to one O(8) atom. The H(9)-O(8) bond length is 0.95 Å. In the eighth H site, H(10) is bonded in a single-bond geometry to one O(8) atom. The H(10)-O(8) bond length is 0.95 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one U(1) 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 water-like geometry to one P(1) and one H(8) 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 distorted bent 150 degrees geometry to one U(2) and one P(2) atom. In the sixth O site, O(6) is bonded in a distorted linear geometry to one U(2) and one P(2) atom. In the seventh O site, O(7) is bonded in a distorted bent 150 degrees geometry to one U(2) and one P(3) atom. In the eighth O site, O(8) is bonded in a distorted trigonal planar geometry to one P(3), one H(10), and one H(9) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one U(1) and one P(3) atom. F(1) is bonded in a distorted bent 120 degrees geometry to two equivalent U(2) atoms. Linkers: 4 [O]P(C[NH](CP(=O)(O)[O])CP(=O)([O])[O])[O].O ,4 [O]P(C[NH](CP(=O)([O])O)CP(=O)([O])[O])[O].O. Metal clusters: 16 [U]. The MOF has largest included sphere 4.97 A, density 2.66 g/cm3, surface area 1888.76 m2/g, accessible volume 0.18 cm3/g