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N2SbBr6 is Fluorite structured and crystallizes in the cubic Fm-3m space group. The structure is zero-dimensional and consists of eight ammonia molecules and four SbBr6 clusters. In each SbBr6 cluster, Sb5+ is bonded in an octahedral geometry to six equivalent Br atoms. All Sb–Br bond lengths are 2.59 Å. Br is bonded in a single-bond geometry to one Sb5+ atom.
C2Sb2NBr7(C2NBr)2 crystallizes in the monoclinic P2_1 space group. The structure is one-dimensional and consists of four C2NBr clusters and one C2Sb2NBr7 ribbon oriented in the (0, 1, 0) direction. In each C2NBr cluster, there are two inequivalent C4+ sites. In the first C4+ site, C4+ is bonded in a single-bond geometry to one N3- atom. The C–N bond length is 1.21 Å. In the second C4+ site, C4+ is bonded in a water-like geometry to one N3- and one Br1- atom. The C–N bond length is 1.33 Å. The C–Br bond length is 1.91 Å. N3- is bonded in a linear geometry to two C4+ atoms. Br1- is bonded in a single-bond geometry to one C4+ atom. In the C2Sb2NBr7 ribbon, there are two inequivalent C4+ sites. In the first C4+ site, C4+ is bonded in a distorted water-like geometry to one N3- and one Br1- atom. The C–N bond length is 1.32 Å. The C–Br bond length is 1.95 Å. In the second C4+ site, C4+ is bonded in a single-bond geometry to one N3- atom. The C–N bond length is 1.21 Å. There are two inequivalent Sb3- sites. In the first Sb3- site, Sb3- is bonded to five Br1- atoms to form distorted corner-sharing SbBr5 trigonal bipyramids. There are a spread of Sb–Br bond distances ranging from 2.64–3.01 Å. In the second Sb3- site, Sb3- is bonded in a distorted rectangular see-saw-like geometry to four Br1- atoms. There are a spread of Sb–Br bond distances ranging from 2.53–3.16 Å. N3- is bonded in a linear geometry to two C4+ atoms. There are seven inequivalent Br1- sites. In the first Br1- site, Br1- is bonded in a single-bond geometry to one Sb3- atom. In the second Br1- site, Br1- is bonded in a distorted bent 120 degrees geometry to one C4+ and one Sb3- atom. In the third Br1- site, Br1- is bonded in a single-bond geometry to one Sb3- atom. In the fourth Br1- site, Br1- is bonded in a bent 150 degrees geometry to two equivalent Sb3- atoms. In the fifth Br1- site, Br1- is bonded in a single-bond geometry to one Sb3- atom. In the sixth Br1- site, Br1- is bonded in a distorted linear geometry to two Sb3- atoms. In the seventh Br1- site, Br1- is bonded in a single-bond geometry to one Sb3- atom.