C7Bi2NH3O6 crystallizes in the monoclinic P2_1 space group. There are seven inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one N(1) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(6) bond length is 1.51 Å. The C(1)-N(1) bond length is 1.35 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1) and one H(1) atom. The C(2)-H(1) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(4) and one H(2) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-H(2) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(7) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-C(7) bond length is 1.51 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4), one N(1), and one H(3) atom. The C(5)-N(1) bond length is 1.34 Å. The C(5)-H(3) 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(1), and one O(2) atom. The C(6)-O(1) bond length is 1.25 Å. The C(6)-O(2) bond length is 1.29 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(7)-O(3) bond length is 1.28 Å. The C(7)-O(4) bond length is 1.27 Å. There are two inequivalent Bi sites. In the first Bi site, Bi(1) is bonded in a 6-coordinate geometry to one O(1), one O(2), one O(3), one O(6), and two equivalent O(5) atoms. The Bi(1)-O(1) bond length is 2.56 Å. The Bi(1)-O(2) bond length is 2.47 Å. The Bi(1)-O(3) bond length is 2.51 Å. The Bi(1)-O(6) bond length is 2.50 Å. There is one shorter (2.16 Å) and one longer (2.42 Å) Bi(1)-O(5) bond length. In the second Bi site, Bi(2) is bonded in a 6-coordinate geometry to one O(2), one O(4), one O(5), and three equivalent O(6) atoms. The Bi(2)-O(2) bond length is 2.76 Å. The Bi(2)-O(4) bond length is 2.76 Å. The Bi(2)-O(5) bond length is 2.14 Å. There is one shorter (2.22 Å) and two longer (2.33 Å) Bi(2)-O(6) bond lengths. N(1) is bonded in a bent 120 degrees geometry to one C(1) and one C(5) atom. There are three 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(3) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(5) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one C(6) and one Bi(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one C(6), one Bi(1), and one Bi(2) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one C(7) and one Bi(1) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(7) and one Bi(2) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Bi(2) and two equivalent Bi(1) atoms. In the sixth O site, O(6) is bonded to one Bi(1) and three equivalent Bi(2) atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. Linkers: 2 [O]C(=O)c1ccc(C([O])=O)nc1. Metal clusters: 4 [Bi]. The MOF has largest included sphere 1.57 A, density 4.36 g/cm3, surface area 1410.02 m2/g, accessible volume 0.03 cm3/g