Na3YbC16N3H8O16(CH)5 crystallizes in the triclinic P-1 space group. The structure consists of ten 02329_fluka molecules inside a Na3YbC16N3H8O16 framework. In the Na3YbC16N3H8O16 framework, there are three inequivalent Na sites. In the first Na site, Na(1) is bonded in a rectangular see-saw-like geometry to one O(13), one O(14), one O(2), and one O(6) atom. The Na(1)-O(13) bond length is 2.29 Å. The Na(1)-O(14) bond length is 2.34 Å. The Na(1)-O(2) bond length is 2.28 Å. The Na(1)-O(6) bond length is 2.36 Å. In the second Na site, Na(2) is bonded in a distorted T-shaped geometry to one O(10), one O(16), and one O(3) atom. The Na(2)-O(10) bond length is 2.30 Å. The Na(2)-O(16) bond length is 2.67 Å. The Na(2)-O(3) bond length is 2.33 Å. In the third Na site, Na(3) is bonded in a distorted trigonal pyramidal geometry to one O(11), one O(15), one O(16), and one O(7) atom. The Na(3)-O(11) bond length is 2.34 Å. The Na(3)-O(15) bond length is 2.31 Å. The Na(3)-O(16) bond length is 2.42 Å. The Na(3)-O(7) bond length is 2.23 Å. Yb(1) is bonded in a 9-coordinate geometry to one N(1), one N(2), one N(3), one O(1), one O(12), one O(4), one O(5), one O(8), and one O(9) atom. The Yb(1)-N(1) bond length is 2.43 Å. The Yb(1)-N(2) bond length is 2.44 Å. The Yb(1)-N(3) bond length is 2.43 Å. The Yb(1)-O(1) bond length is 2.38 Å. The Yb(1)-O(12) bond length is 2.36 Å. The Yb(1)-O(4) bond length is 2.36 Å. The Yb(1)-O(5) bond length is 2.38 Å. The Yb(1)-O(8) bond length is 2.35 Å. The Yb(1)-O(9) bond length is 2.34 Å. There are sixteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one C(7), and one N(1) atom. The C(1)-C(2) bond length is 1.38 Å. The C(1)-C(7) bond length is 1.52 Å. The C(1)-N(1) bond length is 1.34 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 0.93 Å. In the third C site, C(5) is bonded in a distorted single-bond geometry to one N(1) atom. The C(5)-N(1) bond length is 1.31 Å. In the fourth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(6)-O(1) bond length is 1.28 Å. The C(6)-O(2) bond length is 1.24 Å. In the fifth C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(3), and one O(4) atom. The C(7)-O(3) bond length is 1.22 Å. The C(7)-O(4) bond length is 1.28 Å. In the sixth C site, C(8) is bonded in a distorted trigonal planar geometry to one C(14), one C(9), and one N(2) atom. The C(8)-C(14) bond length is 1.50 Å. The C(8)-C(9) bond length is 1.37 Å. The C(8)-N(2) bond length is 1.32 Å. In the seventh C site, C(9) is bonded in a distorted single-bond geometry to one C(8) and one H(4) atom. The C(9)-H(4) bond length is 0.93 Å. In the eighth C site, C(11) is bonded in a distorted single-bond geometry to one C(12) and one H(6) atom. The C(11)-C(12) bond length is 1.38 Å. The C(11)-H(6) bond length is 0.93 Å. In the ninth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(11), one C(13), and one N(2) atom. The C(12)-C(13) bond length is 1.51 Å. The C(12)-N(2) bond length is 1.34 Å. In the tenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(12), one O(5), and one O(6) atom. The C(13)-O(5) bond length is 1.27 Å. The C(13)-O(6) bond length is 1.24 Å. In the eleventh C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(7), and one O(8) atom. The C(14)-O(7) bond length is 1.23 Å. The C(14)-O(8) bond length is 1.27 Å. In the twelfth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(16), one C(21), and one N(3) atom. The C(15)-C(16) bond length is 1.38 Å. The C(15)-C(21) bond length is 1.50 Å. The C(15)-N(3) bond length is 1.35 Å. In the thirteenth C site, C(16) is bonded in a distorted single-bond geometry to one C(15) and one H(7) atom. The C(16)-H(7) bond length is 0.93 Å. In the fourteenth C site, C(19) is bonded in a distorted single-bond geometry to one N(3) atom. The C(19)-N(3) bond length is 1.31 Å. In the fifteenth C site, C(20) is bonded in a distorted bent 120 degrees geometry to one O(10) and one O(9) atom. The C(20)-O(10) bond length is 1.21 Å. The C(20)-O(9) bond length is 1.30 Å. In the sixteenth C site, C(21) is bonded in a distorted bent 120 degrees geometry to one C(15), one O(11), and one O(12) atom. The C(21)-O(11) bond length is 1.25 Å. The C(21)-O(12) bond length is 1.28 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Yb(1), one C(1), and one C(5) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Yb(1), one C(12), and one C(8) atom. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Yb(1), one C(15), and one C(19) atom. 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(4) is bonded in a single-bond geometry to one C(9) atom. In the third H site, H(6) is bonded in a single-bond geometry to one C(11) atom. In the fourth H site, H(7) is bonded in a single-bond geometry to one C(16) atom. In the fifth H site, H(10) is bonded in a single-bond geometry to one O(13) atom. The H(10)-O(13) bond length is 0.93 Å. In the sixth H site, H(11) is bonded in a single-bond geometry to one O(14) atom. The H(11)-O(14) bond length is 0.74 Å. In the seventh H site, H(12) is bonded in a single-bond geometry to one O(15) atom. The H(12)-O(15) bond length is 0.88 Å. In the eighth H site, H(13) is bonded in a single-bond geometry to one O(16) atom. The H(13)-O(16) bond length is 0.95 Å. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(6) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Na(1) and one C(6) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Na(2) and one C(7) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(7) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(13) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Na(1) and one C(13) atom. In the seventh O site, O(7) is bonded in a bent 150 degrees geometry to one Na(3) and one C(14) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Yb(1) and one C(14) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Yb(1) and one C(20) atom. In the tenth O site, O(10) is bonded in a bent 150 degrees geometry to one Na(2) and one C(20) atom. In the eleventh O site, O(11) is bonded in a distorted single-bond geometry to one Na(3) and one C(21) atom. In the twelfth O site, O(12) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(21) atom. In the thirteenth O site, O(13) is bonded in a distorted single-bond geometry to one Na(1) and one H(10) atom. In the fourteenth O site, O(14) is bonded in a distorted bent 120 degrees geometry to one Na(1) and one H(11) atom. In the fifteenth O site, O(15) is bonded in a distorted single-bond geometry to one Na(3) and one H(12) atom. In the sixteenth O site, O(16) is bonded in a 3-coordinate geometry to one Na(2), one Na(3), and one H(13) atom. Linkers: 6 [O]C(=O)c1cccc(C([O])=O)n1 ,2 [OH]. Metal clusters: 6 [Na] ,2 [Yb]. The MOF has largest included sphere 5.48 A, density 1.39 g/cm3, surface area 3811.50 m2/g, accessible volume 0.22 cm3/g