K3Yb(SO4)3 crystallizes in the monoclinic Cc space group. There are three inequivalent K sites. In the first K site, K(1) is bonded in a 8-coordinate geometry to one O(10), one O(2), one O(3), one O(4), one O(6), one O(8), and two equivalent O(12) atoms. In the second K site, K(2) is bonded in a 9-coordinate geometry to one O(10), one O(2), one O(4), one O(5), one O(6), two equivalent O(1), and two equivalent O(9) atoms. In the third K site, K(3) is bonded in a 7-coordinate geometry to one O(5), one O(6), one O(7), one O(8), one O(9), and two equivalent O(11) atoms. Yb(1) is bonded in a 6-coordinate geometry to one O(1), one O(11), one O(12), one O(2), one O(4), and one O(5) atom. There are three inequivalent S sites. In the first S site, S(1) is bonded in a tetrahedral geometry to one O(11), one O(3), one O(6), and one O(7) atom. In the second S site, S(2) is bonded in a trigonal non-coplanar geometry to one O(12), one O(4), and one O(9) atom. In the third S site, S(3) is bonded in a tetrahedral geometry to one O(1), one O(10), one O(5), and one O(8) atom. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent K(2), one Yb(1), and one S(3) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one K(1), one K(2), one Yb(1), and one O(3) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one K(1), one S(1), and one O(2) atom. In the fourth O site, O(4) is bonded in a 4-coordinate geometry to one K(1), one K(2), one Yb(1), and one S(2) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one K(2), one K(3), one Yb(1), and one S(3) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one K(1), one K(2), one K(3), and one S(1) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one K(3) and one S(1) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one K(1), one K(3), and one S(3) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one K(3), two equivalent K(2), and one S(2) atom. In the tenth O site, O(10) is bonded in a distorted single-bond geometry to one K(1), one K(2), and one S(3) atom. In the eleventh O site, O(11) is bonded in a 4-coordinate geometry to two equivalent K(3), one Yb(1), and one S(1) atom. In the twelfth O site, O(12) is bonded in a 2-coordinate geometry to two equivalent K(1), one Yb(1), and one S(2) atom.
K3Yb(SO4)3 crystallizes in the monoclinic Cc space group. There are three inequivalent K sites. In the first K site, K(1) is bonded in a 8-coordinate geometry to one O(10), one O(2), one O(3), one O(4), one O(6), one O(8), and two equivalent O(12) atoms. The K(1)-O(10) bond length is 2.68 Å. The K(1)-O(2) bond length is 3.25 Å. The K(1)-O(3) bond length is 2.97 Å. The K(1)-O(4) bond length is 2.84 Å. The K(1)-O(6) bond length is 2.91 Å. The K(1)-O(8) bond length is 2.72 Å. There is one shorter (3.29 Å) and one longer (3.34 Å) K(1)-O(12) bond length. In the second K site, K(2) is bonded in a 9-coordinate geometry to one O(10), one O(2), one O(4), one O(5), one O(6), two equivalent O(1), and two equivalent O(9) atoms. The K(2)-O(10) bond length is 2.73 Å. The K(2)-O(2) bond length is 3.33 Å. The K(2)-O(4) bond length is 3.19 Å. The K(2)-O(5) bond length is 3.28 Å. The K(2)-O(6) bond length is 3.12 Å. There is one shorter (2.88 Å) and one longer (3.09 Å) K(2)-O(1) bond length. There is one shorter (2.95 Å) and one longer (3.33 Å) K(2)-O(9) bond length. In the third K site, K(3) is bonded in a 7-coordinate geometry to one O(5), one O(6), one O(7), one O(8), one O(9), and two equivalent O(11) atoms. The K(3)-O(5) bond length is 2.75 Å. The K(3)-O(6) bond length is 3.00 Å. The K(3)-O(7) bond length is 3.11 Å. The K(3)-O(8) bond length is 2.80 Å. The K(3)-O(9) bond length is 2.78 Å. There is one shorter (2.71 Å) and one longer (2.79 Å) K(3)-O(11) bond length. Yb(1) is bonded in a 6-coordinate geometry to one O(1), one O(11), one O(12), one O(2), one O(4), and one O(5) atom. The Yb(1)-O(1) bond length is 2.34 Å. The Yb(1)-O(11) bond length is 2.45 Å. The Yb(1)-O(12) bond length is 2.38 Å. The Yb(1)-O(2) bond length is 2.46 Å. The Yb(1)-O(4) bond length is 2.35 Å. The Yb(1)-O(5) bond length is 2.27 Å. There are three inequivalent S sites. In the first S site, S(1) is bonded in a tetrahedral geometry to one O(11), one O(3), one O(6), and one O(7) atom. The S(1)-O(11) bond length is 1.48 Å. The S(1)-O(3) bond length is 1.64 Å. The S(1)-O(6) bond length is 1.46 Å. The S(1)-O(7) bond length is 1.45 Å. In the second S site, S(2) is bonded in a trigonal non-coplanar geometry to one O(12), one O(4), and one O(9) atom. The S(2)-O(12) bond length is 1.51 Å. The S(2)-O(4) bond length is 1.53 Å. The S(2)-O(9) bond length is 1.50 Å. In the third S site, S(3) is bonded in a tetrahedral geometry to one O(1), one O(10), one O(5), and one O(8) atom. The S(3)-O(1) bond length is 1.51 Å. The S(3)-O(10) bond length is 1.48 Å. The S(3)-O(5) bond length is 1.50 Å. The S(3)-O(8) bond length is 1.48 Å. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent K(2), one Yb(1), and one S(3) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one K(1), one K(2), one Yb(1), and one O(3) atom. The O(2)-O(3) bond length is 1.46 Å. In the third O site, O(3) is bonded in a distorted single-bond geometry to one K(1), one S(1), and one O(2) atom. In the fourth O site, O(4) is bonded in a 4-coordinate geometry to one K(1), one K(2), one Yb(1), and one S(2) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one K(2), one K(3), one Yb(1), and one S(3) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one K(1), one K(2), one K(3), and one S(1) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one K(3) and one S(1) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one K(1), one K(3), and one S(3) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one K(3), two equivalent K(2), and one S(2) atom. In the tenth O site, O(10) is bonded in a distorted single-bond geometry to one K(1), one K(2), and one S(3) atom. In the eleventh O site, O(11) is bonded in a 4-coordinate geometry to two equivalent K(3), one Yb(1), and one S(1) atom. In the twelfth O site, O(12) is bonded in a 2-coordinate geometry to two equivalent K(1), one Yb(1), and one S(2) atom.