Cu4SiH12(C2O)16 crystallizes in the tetragonal P4/nmm space group. Cu(1) is bonded in a distorted rectangular see-saw-like geometry to two equivalent O(1) and two equivalent O(2) atoms. Both Cu(1)-O(1) bond lengths are 1.96 Å. Both Cu(1)-O(2) bond lengths are 1.97 Å. Si(1) is bonded in a tetrahedral geometry to four equivalent C(4) atoms. All Si(1)-C(4) bond lengths are 1.88 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(4) bond length is 1.40 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(5) atom. The C(2)-C(3) bond length is 1.49 Å. The C(2)-C(5) bond length is 1.38 Å. In the third C site, C(3) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.24 Å. The C(3)-O(2) bond length is 1.25 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one Si(1) and two equivalent C(1) atoms. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to two equivalent C(2) and one H(2) atom. The C(5)-H(2) bond length is 0.93 Å. There are two 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(5) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(3) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(3) atom. Linkers: 2 [O]C(=O)c1cc(C([O])=O)cc([Si](c2cc(C([O])=O)cc(C([O])=O)c2)(c2cc(C([O])=O)cc(C([O])=O)c2)c2cc(C([O])=O)cc(C([O])=O)c2)c1. Metal clusters: 4 [C]1O[Cu]234O[C]O[Cu]2(O1)(O[C]O3)O[C]O4. RCSR code: scu. The MOF has largest included sphere 9.16 A, density 1.11 g/cm3, surface area 3207.57 m2/g, accessible volume 0.58 cm3/g