| Abstrakt: |
The molecular and crystal structures of a pair of quarternised bromide derivatives of hexamethylenetetramine have been determined. 1-(8-Carboxyoctyl)-1,3,5,7-tetraazaadamantan-1-ium bromide, 1, C14H27N4O2Br, Mr= 363.31, triclinic, P1, a= 9.759(5), b= 12.699(7), c= 14.125(6) Å, α = 96.45(3), β = 99.17(3), γ = 104.74(3)°, V= 1649.7(14) Å3, Z= 4, Dc= 1.463 g cm−3, λ(MoKα) = 0.7107 Å, μ = 2.503 cm−1, F(000) = 760, R(on F) = 0.058, RW(on I) = 0.162 for 3625 unique reflections with [I–σ(I)]. There are two symmetry independent sets of ions, each set being linked with strong O⋯Br interactions to form linear arrays. The symmetry indenpendent arrays are in turn connected with CH⋯O interactions to form a layer. 1-(6-Bromohexyl)-1,3,5,7-tetraazaadamantan-1-ium bromide, 2, C12H29N4Br2, Mr= 384.17, monoclinic, P21/n, a= 8.976(4), b= 15.743(8), c= 11.329(6) Å, β = 103.70(2)°, V= 1555.3(13) Å3, Z= 4, Dc= 1.641 g cm−3, λ(MoKα) = 0.7107 Å μ = 5.203 cm−1, F(000) = 776, R(on F) = 0.066, RW(on I) = 0.168 for 1310 unique non-zero reflections with [I⪢ 2σ(I)]. Two Br−anions are located between two cations resulting in the formation of a cyclic centrosymmetric dimer. Each dimer is surrounded by six similar dimers and is connected to them with CH⋯N hydrogen bonds to form corrugated molecular sheets. The symmetrical bond lengths of the hexamethylenetetramine skeleton are distorted by quarternisation in both 1and 2. |
