Yb2CuC24H8(NO2)8 crystallizes in the monoclinic P2_1/c space group. Yb(1) is bonded in a 6-coordinate geometry to one N(2), one N(4), one O(1), one O(2), one O(3), and one O(5) atom. The Yb(1)-N(2) bond length is 2.65 Å. The Yb(1)-N(4) bond length is 2.60 Å. The Yb(1)-O(1) bond length is 2.34 Å. The Yb(1)-O(2) bond length is 2.20 Å. The Yb(1)-O(3) bond length is 2.29 Å. The Yb(1)-O(5) bond length is 2.25 Å. Cu(1) is bonded in a distorted octahedral geometry to two equivalent N(3), two equivalent O(6), and two equivalent O(8) atoms. Both Cu(1)-N(3) bond lengths are 1.99 Å. Both Cu(1)-O(6) bond lengths are 2.46 Å. Both Cu(1)-O(8) bond lengths are 1.95 Å. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(2) atom. The C(1)-N(3) bond length is 1.33 Å. The C(1)-H(2) bond length is 0.93 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(10), one C(5), and one N(3) atom. The C(2)-C(10) bond length is 1.49 Å. The C(2)-C(5) bond length is 1.39 Å. The C(2)-N(3) bond length is 1.35 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(1) atom. The C(3)-N(4) bond length is 1.34 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(4), and one O(5) atom. The C(4)-C(8) bond length is 1.52 Å. The C(4)-O(4) bond length is 1.22 Å. The C(4)-O(5) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(2), one C(7), and one N(1) atom. The C(5)-C(7) bond length is 1.51 Å. The C(5)-N(1) bond length is 1.34 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(4) atom. The C(6)-N(1) bond length is 1.35 Å. The C(6)-H(4) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(2), and one O(6) atom. The C(7)-O(2) bond length is 1.28 Å. The C(7)-O(6) bond length is 1.23 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(4), one C(9), and one N(4) atom. The C(8)-C(9) bond length is 1.39 Å. The C(8)-N(4) bond length is 1.34 Å. In the ninth C site, C(9) is bonded in a distorted trigonal planar geometry to one C(12), one C(8), and one N(2) atom. The C(9)-C(12) bond length is 1.51 Å. The C(9)-N(2) bond length is 1.35 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(7), and one O(8) atom. The C(10)-O(7) bond length is 1.22 Å. The C(10)-O(8) bond length is 1.28 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(3) atom. The C(11)-N(2) bond length is 1.34 Å. The C(11)-H(3) bond length is 0.93 Å. In the twelfth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(1), and one O(3) atom. The C(12)-O(1) bond length is 1.26 Å. The C(12)-O(3) bond length is 1.26 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a bent 120 degrees geometry to one C(5) and one C(6) atom. In the second N site, N(2) is bonded in a distorted bent 120 degrees geometry to one Yb(1), one C(11), and one C(9) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. In the fourth N site, N(4) is bonded in a distorted bent 120 degrees geometry to one Yb(1), one C(3), and one C(8) atom. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(1) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(11) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(12) atom. In the second O site, O(2) is bonded in a distorted linear geometry to one Yb(1) and one C(7) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(12) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(4) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Cu(1) and one C(7) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one C(10) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(10) atom. Linkers: 8 [O]C(=O)c1nccnc1C([O])=O. Metal clusters: 4 [Yb] ,2 [Cu]. The MOF has largest included sphere 5.17 A, density 2.04 g/cm3, surface area 2750.80 m2/g, accessible volume 0.16 cm3/g