DyCoC12H7(NO2)4 crystallizes in the monoclinic C2/c space group. Dy(1) is bonded in a 6-coordinate geometry to one O(2), one O(4), one O(5), one O(6), and two equivalent O(3) atoms. The Dy(1)-O(2) bond length is 2.23 Å. The Dy(1)-O(4) bond length is 2.28 Å. The Dy(1)-O(5) bond length is 2.29 Å. The Dy(1)-O(6) bond length is 2.46 Å. There is one shorter (2.41 Å) and one longer (2.55 Å) Dy(1)-O(3) bond length. Co(1) is bonded in an octahedral geometry to one N(1), one N(2), one N(3), one O(1), one O(7), and one O(8) atom. The Co(1)-N(1) bond length is 2.14 Å. The Co(1)-N(2) bond length is 2.09 Å. The Co(1)-N(3) bond length is 2.09 Å. The Co(1)-O(1) bond length is 2.19 Å. The Co(1)-O(7) bond length is 2.16 Å. The Co(1)-O(8) bond length is 2.12 Å. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(10) and one N(3) atom. The C(1)-C(10) bond length is 1.39 Å. The C(1)-N(3) bond length is 1.36 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(4), one N(1), and one N(4) atom. The C(2)-C(4) bond length is 1.47 Å. The C(2)-N(1) bond length is 1.32 Å. The C(2)-N(4) bond length is 1.35 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(11), one N(2), and one N(3) atom. The C(3)-C(11) bond length is 1.49 Å. The C(3)-N(2) bond length is 1.33 Å. The C(3)-N(3) bond length is 1.33 Å. In the fourth C site, C(4) is bonded in a trigonal non-coplanar geometry to one C(2); one H(6); and two equivalent H(3,5) atoms. The C(4)-H(6) bond length is 0.96 Å. Both C(4)-H(3,5) bond lengths are 0.96 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(6) and one N(1) atom. The C(5)-C(6) bond length is 1.38 Å. The C(5)-N(1) bond length is 1.37 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(8), and one N(4) atom. The C(6)-C(8) bond length is 1.48 Å. The C(6)-N(4) bond length is 1.38 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one O(2) and one O(8) atom. The C(7)-O(2) bond length is 1.26 Å. The C(7)-O(8) bond length is 1.24 Å. In the eighth C site, C(8) is bonded in a bent 120 degrees geometry to one C(6), one O(3), and one O(6) atom. The C(8)-O(3) bond length is 1.27 Å. The C(8)-O(6) bond length is 1.26 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(5) atom. The C(9)-O(1) bond length is 1.25 Å. The C(9)-O(5) bond length is 1.28 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(1), one C(12), and one N(2) atom. The C(10)-C(12) bond length is 1.47 Å. The C(10)-N(2) bond length is 1.37 Å. In the eleventh C site, C(11) is bonded in a trigonal non-coplanar geometry to one C(3); one H(4); and two equivalent H(2,7) atoms. The C(11)-H(4) bond length is 0.96 Å. Both C(11)-H(2,7) bond lengths are 0.96 Å. In the twelfth C site, C(12) is bonded in a bent 120 degrees geometry to one C(10), one O(4), and one O(7) atom. The C(12)-O(4) bond length is 1.27 Å. The C(12)-O(7) bond length is 1.25 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Co(1), one C(2), and one C(5) atom. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Co(1), one C(10), and one C(3) atom. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Co(1), one C(1), and one C(3) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one C(2), one C(6), and one H(1) atom. The N(4)-H(1) bond length is 0.88 Å. There are five inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(4) atom. In the second H site, H(2,7) is bonded in a single-bond geometry to one C(11) atom. In the third H site, H(3,5) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(11) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one C(4) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Co(1) and one C(9) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(7) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to two equivalent Dy(1) and one C(8) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Dy(1) and one C(12) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(9) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Dy(1) and one C(8) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Co(1) and one C(12) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Co(1) and one C(7) atom. Linkers: 4 Cc1nc(C([O])=O)c(C([O])=O)[nH]1 ,1 CC1=NC(C([O])=O)=C(C([O])=O)[N]1 ,3 CC1=N[C](C([O])=O)C(C([O])=O)=N1. Metal clusters: 4 [Dy] ,4 [Co]. The MOF has largest included sphere 5.87 A, density 1.91 g/cm3, surface area 2808.22 m2/g, accessible volume 0.21 cm3/g