Zn2C12H6(NO2)3 crystallizes in the trigonal R-3 space group. There are two inequivalent Zn sites. In the first Zn site, Zn(1) is bonded in a distorted see-saw-like geometry to one N(3), one O(2), one O(4), and one O(6) atom. The Zn(1)-N(3) bond length is 2.07 Å. The Zn(1)-O(2) bond length is 2.07 Å. The Zn(1)-O(4) bond length is 2.01 Å. The Zn(1)-O(6) bond length is 2.00 Å. In the second Zn site, Zn(2) is bonded to one N(1), one O(1), one O(3), and two equivalent O(6) atoms to form edge-sharing ZnNO4 trigonal bipyramids. The Zn(2)-N(1) bond length is 2.00 Å. The Zn(2)-O(1) bond length is 2.10 Å. The Zn(2)-O(3) bond length is 1.99 Å. There is one shorter (2.02 Å) and one longer (2.14 Å) Zn(2)-O(6) bond length. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.24 Å. The C(1)-O(2) bond length is 1.26 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(6) atom. The C(2)-C(3) bond length is 1.38 Å. The C(2)-C(6) bond length is 1.39 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(8), and one H(2) atom. The C(3)-C(8) bond length is 1.39 Å. The C(3)-H(2) 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(5), one O(3), and one O(4) atom. The C(4)-C(5) bond length is 1.51 Å. The C(4)-O(3) bond length is 1.26 Å. The C(4)-O(4) bond length is 1.24 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(7) atom. The C(5)-C(6) bond length is 1.38 Å. The C(5)-C(7) bond length is 1.41 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(2), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(5), one C(8), and one H(4) atom. The C(7)-C(8) bond length is 1.37 Å. The C(7)-H(4) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a distorted trigonal planar geometry to one C(3), one C(7), and one N(2) atom. The C(8)-N(2) bond length is 1.43 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(10), one N(2), and one O(5) atom. The C(9)-C(10) bond length is 1.46 Å. The C(9)-N(2) bond length is 1.38 Å. The C(9)-O(5) bond length is 1.22 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to one C(11), one C(12), and one C(9) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-C(12) bond length is 1.40 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one C(10), one N(3), and one H(5) atom. The C(11)-N(3) bond length is 1.34 Å. The C(11)-H(5) 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(10), one N(1), and one H(6) atom. The C(12)-N(1) bond length is 1.32 Å. The C(12)-H(6) bond length is 0.93 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a 3-coordinate geometry to one Zn(2), one C(12), and one N(3) atom. The N(1)-N(3) bond length is 1.38 Å. In the second N site, N(2) is bonded in a bent 120 degrees geometry to one C(8) and one C(9) atom. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Zn(1), one C(11), and one N(1) atom. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(6) atom. The H(1)-O(6) bond length is 0.95 Å. In the second H site, H(2) is bonded in a single-bond geometry to one C(3) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(7) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(12) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Zn(2) and one C(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Zn(1) and one C(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Zn(2) and one C(4) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Zn(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(9) atom. In the sixth O site, O(6) is bonded to one Zn(1), two equivalent Zn(2), and one H(1) atom to form distorted edge-sharing OZn3H tetrahedra. Linkers: 12 [O]C(=O)c1cc([N]C(=O)C2=CN=N[CH]2)cc(C([O])=O)c1 ,6 [O]C(=O)c1cc([N]C(=O)C2=C[N]N=C2)cc(C([O])=O)c1. Metal clusters: 9 O[Zn@]12/N=N\[Zn]3O[C]O[Zn@](O)(/N=N\[Zn](O[C]O1)O[C]O2)O[C]O3. RCSR code: kgm. The MOF has largest included sphere 11.93 A, density 0.79 g/cm3, surface area 3591.84 m2/g, accessible volume 0.84 cm3/g