Mo6FeRh3N2 crystallizes in the monoclinic P2_1 space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a bent 150 degrees geometry to one Fe(1), one Rh(2), two equivalent Rh(1), two equivalent Rh(3), and two equivalent N(1) atoms. In the second Mo site, Mo(2) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(3), two equivalent Rh(2), and two equivalent N(2) atoms. In the third Mo site, Mo(3) is bonded in a distorted bent 150 degrees geometry to one Fe(1), one Rh(3), two equivalent Rh(1), two equivalent Rh(2), one N(1), and one N(2) atom. In the fourth Mo site, Mo(4) is bonded in a bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(2), two equivalent Rh(3), one N(1), and one N(2) atom. In the fifth Mo site, Mo(5) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(2), two equivalent Rh(3), one N(1), and one N(2) atom. In the sixth Mo site, Mo(6) is bonded in a bent 150 degrees geometry to one Fe(1), one Rh(3), two equivalent Rh(1), two equivalent Rh(2), one N(1), and one N(2) atom. Fe(1) is bonded to one Mo(1), one Mo(3), one Mo(6), two equivalent Mo(2), two equivalent Mo(4), two equivalent Mo(5), one Rh(2), and two equivalent Rh(3) atoms to form distorted FeMo9Rh3 cuboctahedra that share corners with two equivalent Fe(1)Mo9Rh3 cuboctahedra, corners with four equivalent Rh(1)Mo9Rh3 cuboctahedra,  an edgeedge with one N(1)Mo6 octahedra, edges with two equivalent N(2)Mo6 octahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with four equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with two equivalent N(1)Mo6 octahedra, and faces with two equivalent N(2)Mo6 octahedra. There are three inequivalent Rh sites. In the first Rh site, Rh(1) is bonded to one Mo(2), one Mo(4), one Mo(5), two equivalent Mo(1), two equivalent Mo(3), two equivalent Mo(6), one Rh(3), and two equivalent Rh(2) atoms to form RhMo9Rh3 cuboctahedra that share corners with two equivalent Rh(1)Mo9Rh3 cuboctahedra, corners with four equivalent Fe(1)Mo9Rh3 cuboctahedra,  an edgeedge with one N(2)Mo6 octahedra, edges with two equivalent N(1)Mo6 octahedra, faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with four equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with two equivalent N(1)Mo6 octahedra, and faces with two equivalent N(2)Mo6 octahedra. In the second Rh site, Rh(2) is bonded in a 12-coordinate geometry to one Mo(1), one Mo(4), one Mo(5), two equivalent Mo(2), two equivalent Mo(3), two equivalent Mo(6), one Fe(1), and two equivalent Rh(1) atoms. In the third Rh site, Rh(3) is bonded in a 12-coordinate geometry to one Mo(2), one Mo(3), one Mo(6), two equivalent Mo(1), two equivalent Mo(4), two equivalent Mo(5), two equivalent Fe(1), and one Rh(1) atom. There are two inequivalent N sites. In the first N site, N(1) is bonded to one Mo(3), one Mo(4), one Mo(5), one Mo(6), and two equivalent Mo(1) atoms to form distorted NMo6 octahedra that share corners with two equivalent N(1)Mo6 octahedra, corners with four equivalent N(2)Mo6 octahedra,  an edgeedge with one Fe(1)Mo9Rh3 cuboctahedra, edges with two equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, and faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra. The corner-sharing octahedral tilt angles range from 23-26°. In the second N site, N(2) is bonded to one Mo(3), one Mo(4), one Mo(5), one Mo(6), and two equivalent Mo(2) atoms to form distorted NMo6 octahedra that share corners with two equivalent N(2)Mo6 octahedra, corners with four equivalent N(1)Mo6 octahedra,  an edgeedge with one Rh(1)Mo9Rh3 cuboctahedra, edges with two equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, and faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra. The corner-sharing octahedral tilt angles range from 23-26°.
Mo6FeRh3N2 crystallizes in the monoclinic P2_1 space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded in a bent 150 degrees geometry to one Fe(1), one Rh(2), two equivalent Rh(1), two equivalent Rh(3), and two equivalent N(1) atoms. The Mo(1)-Fe(1) bond length is 2.83 Å. The Mo(1)-Rh(2) bond length is 2.82 Å. There is one shorter (2.77 Å) and one longer (2.88 Å) Mo(1)-Rh(1) bond length. There is one shorter (2.82 Å) and one longer (2.92 Å) Mo(1)-Rh(3) bond length. Both Mo(1)-N(1) bond lengths are 2.13 Å. In the second Mo site, Mo(2) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(3), two equivalent Rh(2), and two equivalent N(2) atoms. There is one shorter (2.74 Å) and one longer (2.94 Å) Mo(2)-Fe(1) bond length. The Mo(2)-Rh(1) bond length is 2.84 Å. The Mo(2)-Rh(3) bond length is 2.89 Å. There is one shorter (2.73 Å) and one longer (2.81 Å) Mo(2)-Rh(2) bond length. There is one shorter (2.13 Å) and one longer (2.14 Å) Mo(2)-N(2) bond length. In the third Mo site, Mo(3) is bonded in a distorted bent 150 degrees geometry to one Fe(1), one Rh(3), two equivalent Rh(1), two equivalent Rh(2), one N(1), and one N(2) atom. The Mo(3)-Fe(1) bond length is 2.73 Å. The Mo(3)-Rh(3) bond length is 2.89 Å. There is one shorter (2.86 Å) and one longer (2.94 Å) Mo(3)-Rh(1) bond length. There is one shorter (2.79 Å) and one longer (2.96 Å) Mo(3)-Rh(2) bond length. The Mo(3)-N(1) bond length is 2.13 Å. The Mo(3)-N(2) bond length is 2.13 Å. In the fourth Mo site, Mo(4) is bonded in a bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(2), two equivalent Rh(3), one N(1), and one N(2) atom. There is one shorter (2.81 Å) and one longer (2.86 Å) Mo(4)-Fe(1) bond length. The Mo(4)-Rh(1) bond length is 2.78 Å. The Mo(4)-Rh(2) bond length is 2.82 Å. There is one shorter (2.77 Å) and one longer (2.79 Å) Mo(4)-Rh(3) bond length. The Mo(4)-N(1) bond length is 2.12 Å. The Mo(4)-N(2) bond length is 2.15 Å. In the fifth Mo site, Mo(5) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1), one Rh(1), one Rh(2), two equivalent Rh(3), one N(1), and one N(2) atom. There is one shorter (2.75 Å) and one longer (2.80 Å) Mo(5)-Fe(1) bond length. The Mo(5)-Rh(1) bond length is 2.91 Å. The Mo(5)-Rh(2) bond length is 2.80 Å. There is one shorter (2.80 Å) and one longer (2.86 Å) Mo(5)-Rh(3) bond length. The Mo(5)-N(1) bond length is 2.14 Å. The Mo(5)-N(2) bond length is 2.14 Å. In the sixth Mo site, Mo(6) is bonded in a bent 150 degrees geometry to one Fe(1), one Rh(3), two equivalent Rh(1), two equivalent Rh(2), one N(1), and one N(2) atom. The Mo(6)-Fe(1) bond length is 2.89 Å. The Mo(6)-Rh(3) bond length is 2.76 Å. There is one shorter (2.77 Å) and one longer (2.86 Å) Mo(6)-Rh(1) bond length. There is one shorter (2.85 Å) and one longer (2.98 Å) Mo(6)-Rh(2) bond length. The Mo(6)-N(1) bond length is 2.13 Å. The Mo(6)-N(2) bond length is 2.12 Å. Fe(1) is bonded to one Mo(1), one Mo(3), one Mo(6), two equivalent Mo(2), two equivalent Mo(4), two equivalent Mo(5), one Rh(2), and two equivalent Rh(3) atoms to form distorted FeMo9Rh3 cuboctahedra that share corners with two equivalent Fe(1)Mo9Rh3 cuboctahedra, corners with four equivalent Rh(1)Mo9Rh3 cuboctahedra,  an edgeedge with one N(1)Mo6 octahedra, edges with two equivalent N(2)Mo6 octahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with four equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with two equivalent N(1)Mo6 octahedra, and faces with two equivalent N(2)Mo6 octahedra. The Fe(1)-Rh(2) bond length is 2.49 Å. Both Fe(1)-Rh(3) bond lengths are 2.50 Å. There are three inequivalent Rh sites. In the first Rh site, Rh(1) is bonded to one Mo(2), one Mo(4), one Mo(5), two equivalent Mo(1), two equivalent Mo(3), two equivalent Mo(6), one Rh(3), and two equivalent Rh(2) atoms to form RhMo9Rh3 cuboctahedra that share corners with two equivalent Rh(1)Mo9Rh3 cuboctahedra, corners with four equivalent Fe(1)Mo9Rh3 cuboctahedra,  an edgeedge with one N(2)Mo6 octahedra, edges with two equivalent N(1)Mo6 octahedra, faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with four equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with two equivalent N(1)Mo6 octahedra, and faces with two equivalent N(2)Mo6 octahedra. The Rh(1)-Rh(3) bond length is 2.60 Å. Both Rh(1)-Rh(2) bond lengths are 2.60 Å. In the second Rh site, Rh(2) is bonded in a 12-coordinate geometry to one Mo(1), one Mo(4), one Mo(5), two equivalent Mo(2), two equivalent Mo(3), two equivalent Mo(6), one Fe(1), and two equivalent Rh(1) atoms. In the third Rh site, Rh(3) is bonded in a 12-coordinate geometry to one Mo(2), one Mo(3), one Mo(6), two equivalent Mo(1), two equivalent Mo(4), two equivalent Mo(5), two equivalent Fe(1), and one Rh(1) atom. There are two inequivalent N sites. In the first N site, N(1) is bonded to one Mo(3), one Mo(4), one Mo(5), one Mo(6), and two equivalent Mo(1) atoms to form distorted NMo6 octahedra that share corners with two equivalent N(1)Mo6 octahedra, corners with four equivalent N(2)Mo6 octahedra,  an edgeedge with one Fe(1)Mo9Rh3 cuboctahedra, edges with two equivalent Rh(1)Mo9Rh3 cuboctahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, and faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra. The corner-sharing octahedral tilt angles range from 23-26°. In the second N site, N(2) is bonded to one Mo(3), one Mo(4), one Mo(5), one Mo(6), and two equivalent Mo(2) atoms to form distorted NMo6 octahedra that share corners with two equivalent N(2)Mo6 octahedra, corners with four equivalent N(1)Mo6 octahedra,  an edgeedge with one Rh(1)Mo9Rh3 cuboctahedra, edges with two equivalent Fe(1)Mo9Rh3 cuboctahedra, faces with two equivalent Fe(1)Mo9Rh3 cuboctahedra, and faces with two equivalent Rh(1)Mo9Rh3 cuboctahedra. The corner-sharing octahedral tilt angles range from 23-26°.