C10Bi2H2O9 crystallizes in the triclinic P-1 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(5), and one C(6) atom. The C(1)-C(2) bond length is 1.41 Å. The C(1)-C(5) bond length is 1.39 Å. The C(1)-C(6) bond length is 1.49 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(4) atom. The C(2)-C(3) bond length is 1.50 Å. The C(2)-C(4) bond length is 1.39 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.28 Å. The C(3)-O(2) bond length is 1.28 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(2), one C(9), and one H(1) atom. The C(4)-C(9) bond length is 1.40 Å. The C(4)-H(1) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(1), one C(7), and one H(2) atom. The C(5)-C(7) bond length is 1.40 Å. The C(5)-H(2) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(3), and one O(4) atom. The C(6)-O(3) bond length is 1.25 Å. The C(6)-O(4) bond length is 1.31 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(5), one C(8), and one C(9) atom. The C(7)-C(8) bond length is 1.50 Å. The C(7)-C(9) bond length is 1.41 Å. In the eighth 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 1.29 Å. The C(8)-O(6) bond length is 1.28 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(10), one C(4), and one C(7) atom. The C(9)-C(10) bond length is 1.51 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(8), and one O(9) atom. The C(10)-O(8) bond length is 1.28 Å. The C(10)-O(9) bond length is 1.27 Å. There are two inequivalent Bi sites. In the first Bi site, Bi(1) is bonded in a 5-coordinate geometry to one O(1), one O(3), one O(9), and two equivalent O(7) atoms. The Bi(1)-O(1) bond length is 2.37 Å. The Bi(1)-O(3) bond length is 2.49 Å. The Bi(1)-O(9) bond length is 2.39 Å. There is one shorter (2.17 Å) and one longer (2.25 Å) Bi(1)-O(7) bond length. In the second Bi site, Bi(2) is bonded in a 8-coordinate geometry to one O(2), one O(6), one O(7), one O(8), two equivalent O(4), and two equivalent O(5) atoms. The Bi(2)-O(2) bond length is 2.56 Å. The Bi(2)-O(6) bond length is 2.37 Å. The Bi(2)-O(7) bond length is 2.17 Å. The Bi(2)-O(8) bond length is 2.67 Å. There is one shorter (2.33 Å) and one longer (2.67 Å) Bi(2)-O(4) bond length. There is one shorter (2.74 Å) and one longer (2.75 Å) Bi(2)-O(5) bond length. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one C(3) and one Bi(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one C(3) and one Bi(2) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one C(6) and one Bi(1) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one C(6) and two equivalent Bi(2) atoms. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(8) and two equivalent Bi(2) atoms. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one C(8) and one Bi(2) atom. In the seventh O site, O(7) is bonded in a distorted trigonal planar geometry to one Bi(2) and two equivalent Bi(1) atoms. In the eighth O site, O(8) is bonded in a single-bond geometry to one C(10) and one Bi(2) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one C(10) and one Bi(1) atom. Linkers: 2 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O. Metal clusters: 1 O=[C]O[Bi]O[Bi](O[C]=O)O[C]=O.O=[C]O[Bi]O[Bi](O[C]=O)O[C]=O.[O][C]=O.[O][C]=O. RCSR code: kgd. The MOF has largest included sphere 1.82 A, density 4.09 g/cm3, surface area 1265.82 m2/g, accessible volume 0.02 cm3/g