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NiB crystallizes in the orthorhombic Cmcm space group. The structure is three-dimensional. Ni3+ is bonded in a 7-coordinate geometry to seven equivalent B3- atoms. There are a spread of Ni–B bond distances ranging from 2.10–2.17 Å. B3- is bonded in a 9-coordinate geometry to seven equivalent Ni3+ and two equivalent B3- atoms. Both B–B bond lengths are 1.78 Å.
Ni3B is Cementite structured and crystallizes in the orthorhombic Pnma space group. The structure is three-dimensional. there are two inequivalent Ni1+ sites. In the first Ni1+ site, Ni1+ is bonded in a 3-coordinate geometry to three equivalent B3- atoms. There are a spread of Ni–B bond distances ranging from 2.02–2.30 Å. In the second Ni1+ site, Ni1+ is bonded in a distorted bent 150 degrees geometry to two equivalent B3- atoms. Both Ni–B bond lengths are 2.02 Å. B3- is bonded in a 6-coordinate geometry to eight Ni1+ atoms.
Ni2B is Khatyrkite structured and crystallizes in the tetragonal I4/mcm space group. The structure is three-dimensional. Ni+1.50+ is bonded in a 4-coordinate geometry to four equivalent B3- atoms. All Ni–B bond lengths are 2.13 Å. B3- is bonded in a 10-coordinate geometry to eight equivalent Ni+1.50+ and two equivalent B3- atoms. Both B–B bond lengths are 2.13 Å.
Ni4B3 crystallizes in the monoclinic C2/c space group. The structure is three-dimensional. there are two inequivalent Ni+2.25+ sites. In the first Ni+2.25+ site, Ni+2.25+ is bonded in a 5-coordinate geometry to five B3- atoms. There are a spread of Ni–B bond distances ranging from 2.06–2.15 Å. In the second Ni+2.25+ site, Ni+2.25+ is bonded in a 6-coordinate geometry to six B3- atoms. There are a spread of Ni–B bond distances ranging from 2.08–2.37 Å. There are two inequivalent B3- sites. In the first B3- site, B3- is bonded in a 9-coordinate geometry to seven Ni+2.25+ and two B3- atoms. There is one shorter (1.85 Å) and one longer (1.87 Å) B–B bond length. In the second B3- site, B3- is bonded in a 10-coordinate geometry to eight Ni+2.25+ and two equivalent B3- atoms.
Ni4B3 crystallizes in the orthorhombic Pnma space group. The structure is three-dimensional. there are four inequivalent Ni+2.25+ sites. In the first Ni+2.25+ site, Ni+2.25+ is bonded in a 6-coordinate geometry to six B3- atoms. There are a spread of Ni–B bond distances ranging from 2.12–2.43 Å. In the second Ni+2.25+ site, Ni+2.25+ is bonded to four B3- atoms to form distorted corner-sharing NiB4 tetrahedra. There are a spread of Ni–B bond distances ranging from 2.03–2.10 Å. In the third Ni+2.25+ site, Ni+2.25+ is bonded in a 7-coordinate geometry to seven B3- atoms. There are a spread of Ni–B bond distances ranging from 2.07–2.34 Å. In the fourth Ni+2.25+ site, Ni+2.25+ is bonded in a 6-coordinate geometry to six B3- atoms. There are a spread of Ni–B bond distances ranging from 2.14–2.20 Å. There are three inequivalent B3- sites. In the first B3- site, B3- is bonded in a 9-coordinate geometry to nine Ni+2.25+ atoms. In the second B3- site, B3- is bonded in a 9-coordinate geometry to seven Ni+2.25+ and two equivalent B3- atoms. Both B–B bond lengths are 1.81 Å. In the third B3- site, B3- is bonded in a 9-coordinate geometry to seven Ni+2.25+ and two equivalent B3- atoms. Both B–B bond lengths are 1.78 Å.