YbC12H9(NO2)3 crystallizes in the triclinic P-1 space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 9-coordinate geometry to one H(9), one O(1), one O(10), one O(12), one O(4), one O(5), one O(6), and two equivalent O(9) atoms. The Yb(1)-H(9) bond length is 2.06 Å. The Yb(1)-O(1) bond length is 2.28 Å. The Yb(1)-O(10) bond length is 2.71 Å. The Yb(1)-O(12) bond length is 2.23 Å. The Yb(1)-O(4) bond length is 2.29 Å. The Yb(1)-O(5) bond length is 2.31 Å. The Yb(1)-O(6) bond length is 2.41 Å. There is one shorter (2.34 Å) and one longer (2.53 Å) Yb(1)-O(9) bond length. In the second Yb site, Yb(2) is bonded in a 7-coordinate geometry to one O(10), one O(11), one O(12), one O(2), one O(3), one O(7), and one O(8) atom. The Yb(2)-O(10) bond length is 2.28 Å. The Yb(2)-O(11) bond length is 2.34 Å. The Yb(2)-O(12) bond length is 2.81 Å. The Yb(2)-O(2) bond length is 2.28 Å. The Yb(2)-O(3) bond length is 2.25 Å. The Yb(2)-O(7) bond length is 2.35 Å. The Yb(2)-O(8) bond length is 2.39 Å. There are twenty-four 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 1.25 Å. The C(1)-O(2) bond length is 1.27 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(7) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-C(7) bond length is 1.38 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(4), and one H(13) atom. The C(3)-C(4) bond length is 1.38 Å. The C(3)-H(13) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(14) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-H(14) bond length is 0.93 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(8) atom. The C(5)-C(6) bond length is 1.42 Å. The C(5)-C(8) bond length is 1.49 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one N(1) atom. The C(6)-C(7) bond length is 1.40 Å. The C(6)-N(1) bond length is 1.38 Å. In the seventh C site, C(7) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one N(2) atom. The C(7)-N(2) bond length is 1.38 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(3), and one O(4) atom. The C(8)-O(3) bond length is 1.27 Å. The C(8)-O(4) bond length is 1.26 Å. In the ninth C site, C(9) is bonded in a bent 120 degrees geometry to one C(10), one O(5), and one O(6) atom. The C(9)-C(10) bond length is 1.49 Å. The C(9)-O(5) bond length is 1.24 Å. The C(9)-O(6) bond length is 1.27 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to one C(11), one C(15), and one C(9) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-C(15) bond length is 1.39 Å. In the eleventh C site, C(11) is bonded in a single-bond geometry to one C(10), one C(12), and one H(15) atom. The C(11)-C(12) bond length is 1.38 Å. The C(11)-H(15) bond length is 0.93 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(11), one C(13), and one N(3) atom. The C(12)-C(13) bond length is 1.40 Å. The C(12)-N(3) bond length is 1.42 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12), one C(14), and one C(16) atom. The C(13)-C(14) bond length is 1.40 Å. The C(13)-C(16) bond length is 1.49 Å. In the fourteenth C site, C(14) is bonded in a distorted single-bond geometry to one C(13), one C(15), and one H(16) atom. The C(14)-C(15) bond length is 1.37 Å. The C(14)-H(16) bond length is 0.93 Å. In the fifteenth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(10), one C(14), and one N(4) atom. The C(15)-N(4) bond length is 1.39 Å. In the sixteenth C site, C(16) is bonded in a bent 120 degrees geometry to one C(13), one O(7), and one O(8) atom. The C(16)-O(7) bond length is 1.26 Å. The C(16)-O(8) bond length is 1.26 Å. In the seventeenth C site, C(17) is bonded in a bent 120 degrees geometry to one C(18), one O(10), and one O(9) atom. The C(17)-C(18) bond length is 1.49 Å. The C(17)-O(10) bond length is 1.26 Å. The C(17)-O(9) bond length is 1.27 Å. In the eighteenth C site, C(18) is bonded in a trigonal planar geometry to one C(17), one C(19), and one C(23) atom. The C(18)-C(19) bond length is 1.40 Å. The C(18)-C(23) bond length is 1.38 Å. In the nineteenth C site, C(19) is bonded in a distorted single-bond geometry to one C(18) and one N(5) atom. The C(19)-N(5) bond length is 1.41 Å. In the twentieth C site, C(20) is bonded in a distorted single-bond geometry to one C(21) and one H(17) atom. The C(20)-C(21) bond length is 1.37 Å. The C(20)-H(17) bond length is 0.93 Å. In the twenty-first C site, C(21) is bonded in a trigonal planar geometry to one C(20), one C(22), and one C(24) atom. The C(21)-C(22) bond length is 1.39 Å. The C(21)-C(24) bond length is 1.50 Å. In the twenty-second C site, C(22) is bonded in a distorted trigonal planar geometry to one C(21), one C(23), and one N(6) atom. The C(22)-C(23) bond length is 1.39 Å. The C(22)-N(6) bond length is 1.38 Å. In the twenty-third C site, C(23) is bonded in a distorted single-bond geometry to one C(18), one C(22), and one H(18) atom. The C(23)-H(18) bond length is 0.93 Å. In the twenty-fourth C site, C(24) is bonded in a bent 120 degrees geometry to one C(21), one O(11), and one O(12) atom. The C(24)-O(11) bond length is 1.26 Å. The C(24)-O(12) bond length is 1.27 Å. There are six inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one C(6) and two equivalent H(1,2) atoms. Both N(1)-H(1,2) bond lengths are 0.86 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one C(7), one H(3), and one H(4) atom. The N(2)-H(3) bond length is 0.86 Å. The N(2)-H(4) bond length is 0.86 Å. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one C(12) and two equivalent H(5,6) atoms. Both N(3)-H(5,6) bond lengths are 0.86 Å. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one C(15), one H(7), and one H(8) atom. The N(4)-H(7) bond length is 0.86 Å. The N(4)-H(8) bond length is 0.86 Å. In the fifth N site, N(5) is bonded in a distorted trigonal planar geometry to one C(19), one H(10), and one H(9) atom. The N(5)-H(10) bond length is 0.86 Å. The N(5)-H(9) bond length is 0.86 Å. In the sixth N site, N(6) is bonded in a distorted trigonal planar geometry to one C(22), one H(11), and one H(12) atom. The N(6)-H(11) bond length is 0.86 Å. The N(6)-H(12) bond length is 0.86 Å. There are sixteen inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one N(1) atom. In the second H site, H(3) is bonded in a single-bond geometry to one N(2) atom. In the third H site, H(4) is bonded in a single-bond geometry to one N(2) atom. In the fourth H site, H(5,6) is bonded in a single-bond geometry to one N(3) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one N(4) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one N(4) atom. In the seventh H site, H(9) is bonded in a distorted single-bond geometry to one Yb(1) and one N(5) atom. In the eighth H site, H(10) is bonded in a single-bond geometry to one N(5) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one N(6) atom. In the tenth H site, H(12) is bonded in a distorted single-bond geometry to one N(6) atom. In the eleventh H site, H(13) is bonded in a single-bond geometry to one C(3) atom. In the twelfth H site, H(14) is bonded in a single-bond geometry to one C(4) atom. In the thirteenth H site, H(15) is bonded in a single-bond geometry to one C(11) atom. In the fourteenth H site, H(16) is bonded in a single-bond geometry to one C(14) atom. In the fifteenth H site, H(17) is bonded in a single-bond geometry to one C(20) atom. In the sixteenth H site, H(18) is bonded in a single-bond geometry to one C(23) atom. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one Yb(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Yb(2) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Yb(2) and one C(8) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one Yb(1) and one C(8) atom. In the fifth O site, O(5) is bonded in a distorted L-shaped geometry to one Yb(1) and one C(9) atom. In the sixth O site, O(6) is bonded in a distorted L-shaped geometry to one Yb(1) and one C(9) atom. In the seventh O site, O(7) is bonded in a distorted L-shaped geometry to one Yb(2) and one C(16) atom. In the eighth O site, O(8) is bonded in a distorted L-shaped geometry to one Yb(2) and one C(16) atom. In the ninth O site, O(9) is bonded in a 1-coordinate geometry to two equivalent Yb(1) and one C(17) atom. In the tenth O site, O(10) is bonded in a 2-coordinate geometry to one Yb(1), one Yb(2), and one C(17) atom. In the eleventh O site, O(11) is bonded in a distorted water-like geometry to one Yb(2) and one C(24) atom. In the twelfth O site, O(12) is bonded in a distorted linear geometry to one Yb(1), one Yb(2), and one C(24) atom. Linkers: 2 Nc1cc(C([O])=O)c(N)cc1C([O])=O ,2 [NH]c1cc(C([O])=O)c(N)cc1C([O])=O ,2 Nc1c(C([O])=O)ccc(C([O])=O)c1N. Metal clusters: 1 O=[C]O[Yb]123O[C]O[Yb]4(O[C]O1)(O[C]O2)(O[C]O3)O[C]O4.O=[C]O[Yb]123O[C]O[Yb]4(O[C]O1)(O[C]O2)(O[C]O3)O[C]O4.[NH2].[NH2]. RCSR code: pcu. The MOF has largest included sphere 4.27 A, density 2.11 g/cm3, surface area 2528.77 m2/g, accessible volume 0.17 cm3/g