NiCdH8(CN)6(CH3CHO)2 crystallizes in the monoclinic C2/c space group. The structure consists of eight dimethyl ether molecules inside a NiCdH8(CN)6 framework. In the NiCdH8(CN)6 framework, Ni(1) is bonded in a square co-planar geometry to two equivalent C(1) and two equivalent C(2) atoms. Both Ni(1)-C(1) bond lengths are 1.83 Å. Both Ni(1)-C(2) bond lengths are 1.84 Å. Cd(1) is bonded in an octahedral geometry to two equivalent N(1), two equivalent N(2), and two equivalent N(3) atoms. Both Cd(1)-N(1) bond lengths are 2.35 Å. Both Cd(1)-N(2) bond lengths are 2.35 Å. Both Cd(1)-N(3) bond lengths are 2.39 Å. There are three inequivalent C sites. In the first C site, C(1) is bonded in a linear geometry to one Ni(1) and one N(1) atom. The C(1)-N(1) bond length is 1.17 Å. In the second C site, C(2) is bonded in a linear geometry to one Ni(1) and one N(2) atom. The C(2)-N(2) bond length is 1.17 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to one N(3), one H(1), and one H(2) atom. The C(3)-N(3) bond length is 1.48 Å. The C(3)-H(1) bond length is 1.10 Å. The C(3)-H(2) bond length is 1.10 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a distorted bent 150 degrees geometry to one Cd(1) and one C(1) atom. In the second N site, N(2) is bonded in a distorted bent 150 degrees geometry to one Cd(1) and one C(2) atom. In the third N site, N(3) is bonded in a 3-coordinate geometry to one Cd(1), one C(3), one H(7), and one H(8) atom. The N(3)-H(7) bond length is 1.02 Å. The N(3)-H(8) bond length is 1.02 Å. There are four inequivalent H sites. In the first H site, H(7) is bonded in a single-bond geometry to one N(3) atom. In the second H site, H(8) is bonded in a single-bond geometry to one N(3) atom. In the third H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(2) is bonded in a single-bond geometry to one C(3) atom. Linkers: 2 NCCOCCOCCN. Metal clusters: 2 [Cd]. The MOF has largest included sphere 2.64 A, density 1.84 g/cm3, surface area 4309.53 m2/g, accessible volume 0.16 cm3/g