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Nb3Os crystallizes in the cubic Pm-3n space group. The structure is three-dimensional. Nb is bonded in a 6-coordinate geometry to two equivalent Nb and four equivalent Os atoms. Both Nb–Nb bond lengths are 2.59 Å. All Nb–Os bond lengths are 2.90 Å. Os is bonded to twelve equivalent Nb atoms to form a mixture of face and edge-sharing OsNb12 cuboctahedra.
NbOs3 crystallizes in the hexagonal P-6m2 space group. The structure is three-dimensional. Nb5+ is bonded in a 6-coordinate geometry to six equivalent Os+1.67- atoms. All Nb–Os bond lengths are 2.91 Å. There are two inequivalent Os+1.67- sites. In the first Os+1.67- site, Os+1.67- is bonded to twelve Os+1.67- atoms to form a mixture of face, edge, and corner-sharing OsOs12 cuboctahedra. There are six shorter (2.67 Å) and six longer (2.78 Å) Os–Os bond lengths. In the second Os+1.67- site, Os+1.67- is bonded to three equivalent Nb5+ and nine Os+1.67- atoms to form OsNb3Os9 cuboctahedra that share corners with eighteen equivalent OsNb3Os9 cuboctahedra, edges with twelve OsOs12 cuboctahedra, and faces with fourteen OsOs12 cuboctahedra. All Os–Os bond lengths are 2.78 Å.
Nb3Os2 crystallizes in the orthorhombic Cmm2 space group. The structure is three-dimensional. there are seven inequivalent Nb sites. In the first Nb site, Nb is bonded in a 6-coordinate geometry to eight Nb and seven Os atoms. There are a spread of Nb–Nb bond distances ranging from 2.75–3.28 Å. There are a spread of Nb–Os bond distances ranging from 2.94–3.27 Å. In the second Nb site, Nb is bonded in a 1-coordinate geometry to three Nb and eight Os atoms. There are two shorter (2.76 Å) and one longer (2.88 Å) Nb–Nb bond lengths. There are a spread of Nb–Os bond distances ranging from 2.85–3.20 Å. In the third Nb site, Nb is bonded in a 4-coordinate geometry to two Nb and five Os atoms. The Nb–Nb bond length is 2.65 Å. There are a spread of Nb–Os bond distances ranging from 2.80–3.12 Å. In the fourth Nb site, Nb is bonded in a 4-coordinate geometry to two Nb and five Os atoms. The Nb–Nb bond length is 2.65 Å. There are a spread of Nb–Os bond distances ranging from 2.80–3.13 Å. In the fifth Nb site, Nb is bonded in a 7-coordinate geometry to four Nb and five Os atoms. Both Nb–Nb bond lengths are 2.55 Å. There are a spread of Nb–Os bond distances ranging from 2.85–2.92 Å. In the sixth Nb site, Nb is bonded in a 2-coordinate geometry to one Nb and seven Os atoms. There are a spread of Nb–Os bond distances ranging from 2.54–2.89 Å. In the seventh Nb site, Nb is bonded in a 7-coordinate geometry to four Nb and five Os atoms. There are a spread of Nb–Os bond distances ranging from 2.85–2.91 Å. There are five inequivalent Os sites. In the first Os site, Os is bonded to six Nb and six Os atoms to form distorted OsNb6Os6 cuboctahedra that share corners with sixteen OsNb9Os3 cuboctahedra, edges with two equivalent OsNb6Os6 cuboctahedra, and faces with four equivalent OsNb9Os3 cuboctahedra. There are four shorter (2.63 Å) and two longer (2.79 Å) Os–Os bond lengths. In the second Os site, Os is bonded to eight Nb and four equivalent Os atoms to form OsNb8Os4 cuboctahedra that share corners with sixteen OsNb9Os3 cuboctahedra, edges with two equivalent OsNb8Os4 cuboctahedra, and faces with four equivalent OsNb9Os3 cuboctahedra. All Os–Os bond lengths are 2.66 Å. In the third Os site, Os is bonded to nine Nb and three Os atoms to form distorted OsNb9Os3 cuboctahedra that share corners with eleven OsNb8Os4 cuboctahedra, edges with three equivalent OsNb9Os3 cuboctahedra, and faces with seven OsNb6Os6 cuboctahedra. There are one shorter (2.68 Å) and one longer (2.86 Å) Os–Os bond lengths. In the fourth Os site, Os is bonded to nine Nb and three Os atoms to form distorted OsNb9Os3 cuboctahedra that share corners with eleven OsNb6Os6 cuboctahedra, edges with three equivalent OsNb9Os3 cuboctahedra, and faces with seven OsNb8Os4 cuboctahedra. There are one shorter (2.63 Å) and one longer (2.84 Å) Os–Os bond lengths. In the fifth Os site, Os is bonded in a distorted linear geometry to nine Nb and five Os atoms.