CaMoF5 crystallizes in the monoclinic C2/c space group. Ca(1) is bonded to one F(1), two equivalent F(2), and four equivalent F(3) atoms to form CaF7 pentagonal bipyramids that share corners with four equivalent Mo(1)F6 octahedra, edges with two equivalent Mo(1)F6 octahedra, and edges with two equivalent Ca(1)F7 pentagonal bipyramids. The corner-sharing octahedral tilt angles range from 3-39°. Mo(1) is bonded to two equivalent F(1), two equivalent F(2), and two equivalent F(3) atoms to form MoF6 octahedra that share corners with two equivalent Mo(1)F6 octahedra, corners with four equivalent Ca(1)F7 pentagonal bipyramids, and edges with two equivalent Ca(1)F7 pentagonal bipyramids. The corner-sharing octahedral tilt angles are 40°. There are three inequivalent F sites. In the first F site, F(1) is bonded in a distorted trigonal planar geometry to one Ca(1) and two equivalent Mo(1) atoms. In the second F site, F(2) is bonded in a linear geometry to one Ca(1) and one Mo(1) atom. In the third F site, F(3) is bonded in a distorted trigonal planar geometry to two equivalent Ca(1) and one Mo(1) atom.
CaMoF5 crystallizes in the monoclinic C2/c space group. Ca(1) is bonded to one F(1), two equivalent F(2), and four equivalent F(3) atoms to form CaF7 pentagonal bipyramids that share corners with four equivalent Mo(1)F6 octahedra, edges with two equivalent Mo(1)F6 octahedra, and edges with two equivalent Ca(1)F7 pentagonal bipyramids. The corner-sharing octahedral tilt angles range from 3-39°. The Ca(1)-F(1) bond length is 2.41 Å. Both Ca(1)-F(2) bond lengths are 2.20 Å. There are two shorter (2.30 Å) and two longer (2.48 Å) Ca(1)-F(3) bond lengths. Mo(1) is bonded to two equivalent F(1), two equivalent F(2), and two equivalent F(3) atoms to form MoF6 octahedra that share corners with two equivalent Mo(1)F6 octahedra, corners with four equivalent Ca(1)F7 pentagonal bipyramids, and edges with two equivalent Ca(1)F7 pentagonal bipyramids. The corner-sharing octahedral tilt angles are 40°. Both Mo(1)-F(1) bond lengths are 2.07 Å. Both Mo(1)-F(2) bond lengths are 2.02 Å. Both Mo(1)-F(3) bond lengths are 2.06 Å. There are three inequivalent F sites. In the first F site, F(1) is bonded in a distorted trigonal planar geometry to one Ca(1) and two equivalent Mo(1) atoms. In the second F site, F(2) is bonded in a linear geometry to one Ca(1) and one Mo(1) atom. In the third F site, F(3) is bonded in a distorted trigonal planar geometry to two equivalent Ca(1) and one Mo(1) atom.