C8BiNH2O6 crystallizes in the orthorhombic Pbcn space group. There are eight inequivalent C sites. In the first C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one C(3), and one N(1) atom. The C(2)-C(1) bond length is 1.50 Å. The C(2)-C(3) bond length is 1.39 Å. The C(2)-N(1) bond length is 1.34 Å. In the second C site, C(6) is bonded in a distorted single-bond geometry to one C(4), one C(7), and one H(2) atom. The C(6)-C(4) bond length is 1.40 Å. The C(6)-C(7) bond length is 1.39 Å. The C(6)-H(2) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-H(1) bond length is 1.09 Å. In the fourth C site, C(7) is bonded in a distorted trigonal planar geometry to one C(6), one C(8), and one N(1) atom. The C(7)-C(8) bond length is 1.51 Å. The C(7)-N(1) bond length is 1.34 Å. In the fifth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(6) atom. The C(4)-C(5) bond length is 1.50 Å. In the sixth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(5), and one O(6) atom. The C(8)-O(5) bond length is 1.25 Å. The C(8)-O(6) bond length is 1.29 Å. In the seventh C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(2) bond length is 1.27 Å. In the eighth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(5)-O(3) bond length is 1.29 Å. The C(5)-O(4) bond length is 1.26 Å. Bi(1) is bonded in a 6-coordinate geometry to one N(1), one O(1), one O(2), one O(3), one O(5), and one O(6) atom. The Bi(1)-N(1) bond length is 2.37 Å. The Bi(1)-O(1) bond length is 2.43 Å. The Bi(1)-O(2) bond length is 2.46 Å. The Bi(1)-O(3) bond length is 2.35 Å. The Bi(1)-O(5) bond length is 2.75 Å. The Bi(1)-O(6) bond length is 2.32 Å. N(1) is bonded in a distorted trigonal planar geometry to one C(2), one C(7), and one Bi(1) atom. There are two 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(6) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one C(1) and one Bi(1) atom. In the second O site, O(5) is bonded in a single-bond geometry to one C(8) and one Bi(1) atom. In the third O site, O(2) is bonded in a distorted single-bond geometry to one C(1) and one Bi(1) atom. In the fourth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one C(8) and one Bi(1) atom. In the fifth O site, O(3) is bonded in a distorted single-bond geometry to one C(5) and one Bi(1) atom. In the sixth O site, O(4) is bonded in a single-bond geometry to one C(5) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)nc(C([O])=O)c1. Metal clusters: 8 [Bi]. The MOF has largest included sphere 1.90 A, density 3.34 g/cm3, surface area 1728.90 m2/g, accessible volume 0.04 cm3/g