KFe(MoO4)2 crystallizes in the trigonal P-3c1 space group. K(1) is bonded to six equivalent O(1) and six equivalent O(2) atoms to form KO12 cuboctahedra that share edges with six equivalent K(1)O12 cuboctahedra, edges with six equivalent Mo(1)O4 tetrahedra, and faces with two equivalent Fe(1)O6 octahedra. Mo(1) is bonded to one O(1) and three equivalent O(2) atoms to form MoO4 tetrahedra that share corners with three equivalent Fe(1)O6 octahedra and edges with three equivalent K(1)O12 cuboctahedra. The corner-sharing octahedral tilt angles are 21°. Fe(1) is bonded to six equivalent O(2) atoms to form FeO6 octahedra that share corners with six equivalent Mo(1)O4 tetrahedra and faces with two equivalent K(1)O12 cuboctahedra. There are two inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to three equivalent K(1) and one Mo(1) atom. In the second O site, O(2) is bonded in a distorted bent 150 degrees geometry to one K(1), one Mo(1), and one Fe(1) atom.
KFe(MoO4)2 crystallizes in the trigonal P-3c1 space group. K(1) is bonded to six equivalent O(1) and six equivalent O(2) atoms to form KO12 cuboctahedra that share edges with six equivalent K(1)O12 cuboctahedra, edges with six equivalent Mo(1)O4 tetrahedra, and faces with two equivalent Fe(1)O6 octahedra. All K(1)-O(1) bond lengths are 3.33 Å. All K(1)-O(2) bond lengths are 2.98 Å. Mo(1) is bonded to one O(1) and three equivalent O(2) atoms to form MoO4 tetrahedra that share corners with three equivalent Fe(1)O6 octahedra and edges with three equivalent K(1)O12 cuboctahedra. The corner-sharing octahedral tilt angles are 21°. The Mo(1)-O(1) bond length is 1.75 Å. All Mo(1)-O(2) bond lengths are 1.81 Å. Fe(1) is bonded to six equivalent O(2) atoms to form FeO6 octahedra that share corners with six equivalent Mo(1)O4 tetrahedra and faces with two equivalent K(1)O12 cuboctahedra. All Fe(1)-O(2) bond lengths are 2.01 Å. There are two inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to three equivalent K(1) and one Mo(1) atom. In the second O site, O(2) is bonded in a distorted bent 150 degrees geometry to one K(1), one Mo(1), and one Fe(1) atom.