C10BiNH8O10 crystallizes in the monoclinic Pc space group. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(6) bond length is 1.40 Å. The C(1)-C(7) bond length is 1.48 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-H(1) bond length is 1.09 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-C(8) bond length is 1.49 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(2) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-H(2) bond length is 1.09 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(9) atom. The C(5)-C(6) bond length is 1.40 Å. The C(5)-C(9) bond length is 1.49 Å. In the sixth C site, C(6) is bonded in a distorted trigonal planar geometry to one C(1), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 1.09 Å. In the seventh C site, C(7) is bonded in a bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(7)-O(1) bond length is 1.29 Å. The C(7)-O(2) bond length is 1.27 Å. In the eighth C site, C(8) is bonded in a bent 120 degrees geometry to one C(3), 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 1.29 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(5), and one O(6) atom. The C(9)-O(5) bond length is 1.24 Å. The C(9)-O(6) bond length is 1.34 Å. In the tenth C site, C(10) is bonded in a tetrahedral geometry to one H(6), one H(7), one H(8), and one O(7) atom. The C(10)-H(6) bond length is 1.10 Å. The C(10)-H(7) bond length is 1.09 Å. The C(10)-H(8) bond length is 1.10 Å. The C(10)-O(7) bond length is 1.45 Å. Bi(1) is bonded in a 9-coordinate geometry to one O(1), one O(10), one O(2), one O(3), one O(4), one O(5), one O(7), and two equivalent O(8) atoms. The Bi(1)-O(1) bond length is 2.44 Å. The Bi(1)-O(10) bond length is 2.60 Å. The Bi(1)-O(2) bond length is 2.67 Å. The Bi(1)-O(3) bond length is 2.54 Å. The Bi(1)-O(4) bond length is 2.32 Å. The Bi(1)-O(5) bond length is 2.75 Å. The Bi(1)-O(7) bond length is 2.41 Å. There is one shorter (2.52 Å) and one longer (2.76 Å) Bi(1)-O(8) bond length. N(1) is bonded in a trigonal planar geometry to one O(10), one O(8), and one O(9) atom. The N(1)-O(10) bond length is 1.26 Å. The N(1)-O(8) bond length is 1.32 Å. The N(1)-O(9) bond length is 1.23 Å. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) 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 bent 150 degrees geometry to one O(2) and one O(6) atom. The H(4)-O(2) bond length is 1.63 Å. The H(4)-O(6) bond length is 1.01 Å. In the fifth H site, H(5) is bonded in a distorted single-bond geometry to one O(1) and one O(7) atom. The H(5)-O(1) bond length is 1.66 Å. The H(5)-O(7) bond length is 1.00 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(10) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(10) atom. There are ten inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one C(7), one Bi(1), and one H(5) atom. In the second O site, O(2) is bonded in a 2-coordinate geometry to one C(7), one Bi(1), and one H(4) atom. In the third O site, O(3) is bonded in a single-bond geometry to one C(8) and one Bi(1) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one C(8) and one Bi(1) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(9) and one Bi(1) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one C(9) and one H(4) atom. In the seventh O site, O(7) is bonded in a 2-coordinate geometry to one C(10), one Bi(1), and one H(5) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to two equivalent Bi(1) and one N(1) atom. In the ninth O site, O(9) is bonded in a single-bond geometry to one N(1) atom. In the tenth O site, O(10) is bonded in a distorted single-bond geometry to one Bi(1) and one N(1) atom. Linkers: 2 [O]C(=O)c1cc(C([O])=O)cc(C(=O)O)c1. Metal clusters: 2 CO.O=[C]O[Bi]O[C]=O.[O][N+](=O)[O-]. The MOF has largest included sphere 3.42 A, density 2.25 g/cm3, surface area 2859.48 m2/g, accessible volume 0.11 cm3/g