YbC2PH6O7 crystallizes in the orthorhombic Pnma space group. Yb(1) is bonded to one O(1), one O(2), one O(4), two equivalent O(3), and two equivalent O(5) atoms to form YbO7 pentagonal bipyramids that share corners with three equivalent P(1)CO3 tetrahedra. The Yb(1)-O(1) bond length is 2.32 Å. The Yb(1)-O(2) bond length is 2.24 Å. The Yb(1)-O(4) bond length is 2.12 Å. Both Yb(1)-O(3) bond lengths are 2.18 Å. Both Yb(1)-O(5) bond lengths are 2.42 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted water-like geometry to one P(1) and two equivalent H(3) atoms. The C(1)-P(1) bond length is 1.84 Å. Both C(1)-H(3) bond lengths are 1.10 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to two equivalent O(5) atoms. Both C(2)-O(5) bond lengths are 1.28 Å. P(1) is bonded to one C(1), one O(4), and two equivalent O(3) atoms to form PCO3 tetrahedra that share corners with three equivalent Yb(1)O7 pentagonal bipyramids. The P(1)-O(4) bond length is 1.53 Å. Both P(1)-O(3) bond lengths are 1.53 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(1) atom. The H(1)-O(1) bond length is 0.98 Å. In the second H site, H(2) is bonded in a distorted linear geometry to one O(2) and one O(5) atom. The H(2)-O(2) bond length is 1.00 Å. The H(2)-O(5) bond length is 1.62 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(1) atom. There are five inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Yb(1) and two equivalent H(1) atoms. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one Yb(1) and two equivalent H(2) atoms. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Yb(1) and one P(1) atom. In the fourth O site, O(4) is bonded in a linear geometry to one Yb(1) and one P(1) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one Yb(1), one C(2), and one H(2) atom. Linkers: 4 [O]C(=O)CP([O])([O])=O. Metal clusters: 4 [Yb]. RCSR code: fes. The MOF has largest included sphere 1.98 A, density 3.18 g/cm3, surface area 2011.78 m2/g, accessible volume 0.06 cm3/g