HoC2O4F crystallizes in the monoclinic C2/c space group. Ho(1) is bonded in a 6-coordinate geometry to two equivalent O(1), two equivalent O(2), and two equivalent F(1) atoms. Both Ho(1)-O(1) bond lengths are 2.42 Å. Both Ho(1)-O(2) bond lengths are 2.38 Å. Both Ho(1)-F(1) bond lengths are 2.17 Å. C(1) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.25 Å. There are two inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ho(1) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ho(1) and one C(1) atom. F(1) is bonded in a linear geometry to two equivalent Ho(1) atoms. Linkers: 2 [O]C(=O)C([O])=O. Metal clusters: 2 [Ho]. The MOF has largest included sphere 4.57 A, density 2.12 g/cm3, surface area 2052.48 m2/g, accessible volume 0.27 cm3/g