Ca3C16H12(NO8)2 crystallizes in the triclinic P-1 space group. There are two inequivalent Ca sites. In the first Ca site, Ca(1) is bonded to one N(1), one O(1), one O(3), one O(5), one O(6), and two equivalent O(2) atoms to form distorted edge-sharing CaNO6 pentagonal bipyramids. The Ca(1)-N(1) bond length is 2.53 Å. The Ca(1)-O(1) bond length is 2.33 Å. The Ca(1)-O(3) bond length is 2.40 Å. The Ca(1)-O(5) bond length is 2.38 Å. The Ca(1)-O(6) bond length is 2.44 Å. There is one shorter (2.46 Å) and one longer (2.58 Å) Ca(1)-O(2) bond length. In the second Ca site, Ca(2) is bonded in an octahedral geometry to two equivalent O(4), two equivalent O(7), and two equivalent O(8) atoms. Both Ca(2)-O(4) bond lengths are 2.40 Å. Both Ca(2)-O(7) bond lengths are 2.28 Å. Both Ca(2)-O(8) bond lengths are 2.35 Å. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(5), one C(6), and one N(1) atom. The C(1)-C(5) 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 1.34 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(2), and one O(4) atom. The C(2)-C(3) bond length is 1.51 Å. The C(2)-O(2) bond length is 1.27 Å. The C(2)-O(4) bond length is 1.27 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(8), and one N(1) atom. The C(3)-C(8) bond length is 1.40 Å. The C(3)-N(1) bond length is 1.34 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(5), one C(7), and one C(8) atom. The C(4)-C(5) bond length is 1.40 Å. The C(4)-C(7) bond length is 1.51 Å. The C(4)-C(8) bond length is 1.40 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(1), one C(4), and one H(1) atom. The C(5)-H(1) 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(6), and one O(7) atom. The C(6)-O(6) bond length is 1.28 Å. The C(6)-O(7) bond length is 1.26 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(1), and one O(5) atom. The C(7)-O(1) bond length is 1.26 Å. The C(7)-O(5) bond length is 1.28 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(3), one C(4), and one H(2) atom. The C(8)-H(2) bond length is 1.09 Å. N(1) is bonded in a distorted trigonal planar geometry to one Ca(1), one C(1), and one C(3) atom. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(5) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(8) atom. In the third H site, H(3) is bonded in a single-bond geometry to one O(3) and one O(4) atom. The H(3)-O(3) bond length is 1.00 Å. The H(3)-O(4) bond length is 1.74 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(3) and one O(6) atom. The H(4)-O(3) bond length is 1.01 Å. The H(4)-O(6) bond length is 1.68 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(8) atom. The H(5)-O(8) bond length is 0.99 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(8) atom. The H(6)-O(8) bond length is 1.00 Å. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one Ca(1) and one C(7) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to two equivalent Ca(1) and one C(2) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Ca(1), one H(3), and one H(4) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Ca(2), one C(2), and one H(3) atom. In the fifth O site, O(5) is bonded in a 2-coordinate geometry to one Ca(1) and one C(7) atom. In the sixth O site, O(6) is bonded in a distorted trigonal planar geometry to one Ca(1), one C(6), and one H(4) atom. In the seventh O site, O(7) is bonded in a bent 150 degrees geometry to one Ca(2) and one C(6) atom. In the eighth O site, O(8) is bonded in a distorted water-like geometry to one Ca(2), one H(5), and one H(6) atom. Linkers: 2 [O]C(=O)c1cc(C([O])=O)nc(C([O])=O)c1. Metal clusters: 3 [Ca]. The MOF has largest included sphere 2.29 A, density 1.88 g/cm3, surface area 2981.09 m2/g, accessible volume 0.10 cm3/g