AuCu2C6H12(N2O)2 crystallizes in the monoclinic P2/c space group. There are two inequivalent Au sites. In the first Au site, Au(1) is bonded in a linear geometry to two equivalent C(1) atoms. Both Au(1)-C(1) bond lengths are 1.99 Å. In the second Au site, Au(2) is bonded in a linear geometry to two equivalent C(2) atoms. Both Au(2)-C(2) bond lengths are 1.98 Å. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a 5-coordinate geometry to one N(1), one N(4), one O(1), and two equivalent O(2) atoms. The Cu(1)-N(1) bond length is 1.97 Å. The Cu(1)-N(4) bond length is 2.01 Å. The Cu(1)-O(1) bond length is 1.93 Å. There is one shorter (1.95 Å) and one longer (2.48 Å) Cu(1)-O(2) bond length. In the second Cu site, Cu(2) is bonded in a distorted square co-planar geometry to one N(2), one N(3), one O(1), and one O(2) atom. The Cu(2)-N(2) bond length is 1.97 Å. The Cu(2)-N(3) bond length is 2.04 Å. The Cu(2)-O(1) bond length is 1.94 Å. The Cu(2)-O(2) bond length is 1.98 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a single-bond geometry to one Au(1) and one N(1) atom. The C(1)-N(1) bond length is 1.15 Å. In the second C site, C(2) is bonded in a single-bond geometry to one Au(2) and one N(2) atom. The C(2)-N(2) bond length is 1.15 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to two equivalent H(1,2) and one O(2) atom. Both C(3)-H(1,2) bond lengths are 0.97 Å. The C(3)-O(2) bond length is 1.42 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one N(4) and two equivalent H(3,4) atoms. The C(4)-N(4) bond length is 1.49 Å. Both C(4)-H(3,4) bond lengths are 0.97 Å. In the fifth C site, C(5) is bonded in a distorted trigonal non-coplanar geometry to two equivalent H(7,8) and one O(1) atom. Both C(5)-H(7,8) bond lengths are 0.97 Å. The C(5)-O(1) bond length is 1.42 Å. In the sixth C site, C(6) is bonded in a 3-coordinate geometry to one N(3) and two equivalent H(9,10) atoms. The C(6)-N(3) bond length is 1.49 Å. Both C(6)-H(9,10) bond lengths are 0.97 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a linear geometry to one Cu(1) and one C(1) atom. In the second N site, N(2) is bonded in a linear geometry to one Cu(2) and one C(2) atom. In the third N site, N(3) is bonded in a distorted water-like geometry to one Cu(2); one C(6); and two equivalent H(5,6) atoms. Both N(3)-H(5,6) bond lengths are 0.90 Å. In the fourth N site, N(4) is bonded in a distorted water-like geometry to one Cu(1); one C(4); and two equivalent H(11,12) atoms. Both N(4)-H(11,12) bond lengths are 0.90 Å. There are six inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(3,4) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(5,6) is bonded in a single-bond geometry to one N(3) atom. In the fourth H site, H(7,8) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(9,10) is bonded in a single-bond geometry to one C(6) atom. In the sixth H site, H(11,12) is bonded in a single-bond geometry to one N(4) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal non-coplanar geometry to one Cu(1), one Cu(2), and one C(5) atom. In the second O site, O(2) is bonded in a 4-coordinate geometry to one Cu(2), two equivalent Cu(1), and one C(3) atom. Linkers: 8 NCC[O]. Metal clusters: 8 [Cu] ,4 [Au]. The MOF has largest included sphere 4.31 A, density 2.13 g/cm3, surface area 2709.94 m2/g, accessible volume 0.22 cm3/g