N,N,N',N'-四[2-(1-乙基苯并咪唑)甲基]乙二胺及其高氯酸盐的晶体结构

Crystal Structures of EtEDTB1.4C_2H_5OH5H_2O and H_4EtEDTB(ClO_4)_4C_2H_5OH (EtEDTB=N, N, N' N'- Tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine)

本文通过单晶X-射线衍射法测定了EtEDTB1.4C2H5OH5H2O 1和H4EtEDTB(ClO4)4 C2H5OH 2的晶体结构。晶体学数据如下:1的分子式为C44.8H66.4N10O6.4, Mr = 847.48, 属三斜晶系, 空间群P, a = 11.489 (2), b = 11.866(3), c = 12.002(3) , = 97.47(2), ?= 114.564(13), ?= 114.11(2)? V = 1266.6(5) 3, Z = 1, Dc = 1.111 g/cm3, F(000) = 456, m(MoK? = 0.076 mm-1。共收集衍射数据5207条, 其中独立衍射数据4323条(Rint = 0.0257), 1318条可观测衍射数据(I > 2(I))用于结构计算。结构由直接法解出, 并用全矩阵最小二乘法修正, 最终偏离因子R = 0.0706, wR = 0.1802。分子具有对称中心, 4个苯并咪唑基团围绕中心呈螺旋桨状均匀排布。在1的晶体中, EtEDTB分子通过水和乙醇的氢键相连形成二维网状结构。2的分子式为C44H58Cl4N10O17, Mr = 1140.80, 属单斜晶系, 空间群C2/c, a = 24.260(5), b = 13.040(3), c = 17.680(4) , ?= 97.50(3)? V = 5545.2(2) 3, Z = 4, Dc = 1.366 g/cm3, F(000) = 2384, m(MoK? = 0.289 mm-1。共收集衍射数据12055条, 其中独立衍射数据6360条(Rint = 0.0408), 2875条可观测衍射数据(I > 2(I))用于结构计算。结构由直接法解出, 并用全矩阵最小二乘法修正, 最终偏离因子R = 0.

The crystal structures of EtEDTB1.4C2H5OH5H2O 1 and H4EtEDTB(ClO4)4C2H5OH 2 (EtEDTB = N, N,N?N-tetrakis[2-(1-ethylbenzimidazolyl)methyl]-1,2-ethanediamine) have been determined by single- crystal X-ray diffraction method. Compound 1 crystallizes in the space group P with a = 11.489(2), b = 11.866(3), c = 12.002(3) , = 97.47(2), = 114.564(13), = 114.11(2)? V = 1266.6(5) 3, Z = 1, Mr = 847.48, Dc = 1.111 g/cm3, F(000) = 456 and (MoK? = 0.076 mm-1. A total of 5207 reflections were measured for 1, of which 4323 were independent. The structure of 1 was solved by direct methods and refined by full-matrix least-squares technique to the final R = 0.0706 and wR = 0.1802 for 1318 observed reflections with I > 2(I). In the structure of 1, centrosymmetric EtEDTB molecules are linked by hydrogen bonds through water and ethanol to form 2-dimensional network. Compound 2 crystallizes in the space group C2/c with a = 24.260(5), b = 13.040(3), c = 17.680(4) , = 97.50(3)? V = 5545.2(2) 3, Z = 4, Mr = 1140.80, Dc = 1.366 g/cm3, F(000) = 2384 and (MoK? = 0.289 mm-1. A total of 12055 reflections were measured for 2, of which 6360 were independent. The structure of 2 was also solved by direct methods and refined by full-matrix least-squares technique to the final R = 0.0692 and wR = 0.2098 for 2875 observed reflec- tions with I > 2(I). In the structure of 2, [H4EtEDTB]4+ ion has C2 symmetry, and the two benzimidazolyl- methyl groups bonded to the same amine nitrogen atom are coplanar.