Ni(Mo3Se4)2 crystallizes in the triclinic P1 space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one Se(2), one Se(3), one Se(5), one Se(7), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. In the second Mo site, Mo(2) is bonded to one Se(1), one Se(4), one Se(6), one Se(7), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. In the third Mo site, Mo(3) is bonded to one Se(1), one Se(3), one Se(4), one Se(5), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. In the fourth Mo site, Mo(4) is bonded in a 6-coordinate geometry to one Ni(1), one Se(2), one Se(3), one Se(4), one Se(6), and one Se(7) atom. In the fifth Mo site, Mo(5) is bonded in a 5-coordinate geometry to one Se(1), one Se(2), one Se(4), one Se(5), and one Se(7) atom. In the sixth Mo site, Mo(6) is bonded to one Se(1), one Se(2), one Se(3), one Se(6), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. Ni(1) is bonded in a 4-coordinate geometry to one Mo(4), one Se(2), one Se(3), one Se(4), and one Se(6) atom. There are eight inequivalent Se sites. In the first Se site, Se(1) is bonded in a 4-coordinate geometry to one Mo(2), one Mo(3), one Mo(5), and one Mo(6) atom. In the second Se site, Se(2) is bonded in a 5-coordinate geometry to one Mo(1), one Mo(4), one Mo(5), one Mo(6), and one Ni(1) atom. In the third Se site, Se(3) is bonded in a 5-coordinate geometry to one Mo(1), one Mo(3), one Mo(4), one Mo(6), and one Ni(1) atom. In the fourth Se site, Se(4) is bonded in a 5-coordinate geometry to one Mo(2), one Mo(3), one Mo(4), one Mo(5), and one Ni(1) atom. In the fifth Se site, Se(5) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(3), and one Mo(5) atom. In the sixth Se site, Se(6) is bonded in a 4-coordinate geometry to one Mo(2), one Mo(4), one Mo(6), and one Ni(1) atom. In the seventh Se site, Se(7) is bonded in a distorted rectangular see-saw-like geometry to one Mo(1), one Mo(2), one Mo(4), and one Mo(5) atom. In the eighth Se site, Se(8) is bonded in a distorted rectangular see-saw-like geometry to one Mo(1), one Mo(2), one Mo(3), and one Mo(6) atom.
Ni(Mo3Se4)2 crystallizes in the triclinic P1 space group. There are six inequivalent Mo sites. In the first Mo site, Mo(1) is bonded to one Se(2), one Se(3), one Se(5), one Se(7), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. The Mo(1)-Se(2) bond length is 2.58 Å. The Mo(1)-Se(3) bond length is 2.68 Å. The Mo(1)-Se(5) bond length is 2.54 Å. The Mo(1)-Se(7) bond length is 2.59 Å. The Mo(1)-Se(8) bond length is 2.70 Å. In the second Mo site, Mo(2) is bonded to one Se(1), one Se(4), one Se(6), one Se(7), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. The Mo(2)-Se(1) bond length is 2.54 Å. The Mo(2)-Se(4) bond length is 2.59 Å. The Mo(2)-Se(6) bond length is 2.61 Å. The Mo(2)-Se(7) bond length is 2.71 Å. The Mo(2)-Se(8) bond length is 2.65 Å. In the third Mo site, Mo(3) is bonded to one Se(1), one Se(3), one Se(4), one Se(5), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. The Mo(3)-Se(1) bond length is 2.60 Å. The Mo(3)-Se(3) bond length is 2.63 Å. The Mo(3)-Se(4) bond length is 2.69 Å. The Mo(3)-Se(5) bond length is 2.58 Å. The Mo(3)-Se(8) bond length is 2.56 Å. In the fourth Mo site, Mo(4) is bonded in a 6-coordinate geometry to one Ni(1), one Se(2), one Se(3), one Se(4), one Se(6), and one Se(7) atom. The Mo(4)-Ni(1) bond length is 2.56 Å. The Mo(4)-Se(2) bond length is 2.73 Å. The Mo(4)-Se(3) bond length is 2.71 Å. The Mo(4)-Se(4) bond length is 2.58 Å. The Mo(4)-Se(6) bond length is 2.68 Å. The Mo(4)-Se(7) bond length is 2.54 Å. In the fifth Mo site, Mo(5) is bonded in a 5-coordinate geometry to one Se(1), one Se(2), one Se(4), one Se(5), and one Se(7) atom. The Mo(5)-Se(1) bond length is 2.62 Å. The Mo(5)-Se(2) bond length is 2.68 Å. The Mo(5)-Se(4) bond length is 2.67 Å. The Mo(5)-Se(5) bond length is 2.53 Å. The Mo(5)-Se(7) bond length is 2.61 Å. In the sixth Mo site, Mo(6) is bonded to one Se(1), one Se(2), one Se(3), one Se(6), and one Se(8) atom to form a mixture of distorted corner and edge-sharing MoSe5 square pyramids. The Mo(6)-Se(1) bond length is 2.69 Å. The Mo(6)-Se(2) bond length is 2.63 Å. The Mo(6)-Se(3) bond length is 2.60 Å. The Mo(6)-Se(6) bond length is 2.56 Å. The Mo(6)-Se(8) bond length is 2.60 Å. Ni(1) is bonded in a 4-coordinate geometry to one Mo(4), one Se(2), one Se(3), one Se(4), and one Se(6) atom. The Ni(1)-Se(2) bond length is 2.31 Å. The Ni(1)-Se(3) bond length is 2.48 Å. The Ni(1)-Se(4) bond length is 2.34 Å. The Ni(1)-Se(6) bond length is 2.34 Å. There are eight inequivalent Se sites. In the first Se site, Se(1) is bonded in a 4-coordinate geometry to one Mo(2), one Mo(3), one Mo(5), and one Mo(6) atom. In the second Se site, Se(2) is bonded in a 5-coordinate geometry to one Mo(1), one Mo(4), one Mo(5), one Mo(6), and one Ni(1) atom. In the third Se site, Se(3) is bonded in a 5-coordinate geometry to one Mo(1), one Mo(3), one Mo(4), one Mo(6), and one Ni(1) atom. In the fourth Se site, Se(4) is bonded in a 5-coordinate geometry to one Mo(2), one Mo(3), one Mo(4), one Mo(5), and one Ni(1) atom. In the fifth Se site, Se(5) is bonded in a 3-coordinate geometry to one Mo(1), one Mo(3), and one Mo(5) atom. In the sixth Se site, Se(6) is bonded in a 4-coordinate geometry to one Mo(2), one Mo(4), one Mo(6), and one Ni(1) atom. In the seventh Se site, Se(7) is bonded in a distorted rectangular see-saw-like geometry to one Mo(1), one Mo(2), one Mo(4), and one Mo(5) atom. In the eighth Se site, Se(8) is bonded in a distorted rectangular see-saw-like geometry to one Mo(1), one Mo(2), one Mo(3), and one Mo(6) atom.