三维超分子化合物[H_2(C_4H_(10)N_2)](SO_4)(H_2O)的制备、晶体结构及差热-热重性质研究

用MnSO4H2O和哌嗪在水-甲醇混合溶剂中反应得到了1个超分子化合物H2(C4H10N2)](SO4)(H2O) (C4H14N2O5S)。 该晶体属单斜晶系, 空间群为P21/n, 晶胞参数为: a = 6.386(1), b = 11.695(2), c = 11.680(2) ? = 101.06(3), V = 856.1(3) 3, Z = 4, Mr =202.23 , Dc = 1.569 g/cm3, F(000) = 432, ?= 0.368 mm-1。 该化合物是由H2(C4H10N2)]2+、SO42-、H2O通过氢键自组装而形成的。 其中H2(C4H10N2)]2+存在2种椅式构象:一种H2(C4H10N2)]2+与4个SO42-、2个H2O通过氢键相连, 另一种H2(C4H10N2)]2+则与6个SO42-相连。 它们分别沿着b、c方向交替排列展开, 通过SO42-桥联成二维的层状结构;层与层之间在NH…O、CH…O、OH…O氢键的作用下互相连接, 形成了具有网状结构的三维超分子化合物。 差热及热重测试表明:该化合物从92℃开始分解,首先失去1个H2O, 然后再失去H2(C4H10N2)]2+和SO4 2-。

Synthesis, Crystal Structure and Thermal Property of Three-dimensional Supramolecular Compound [(C4H12N2)(SO4)(H2O)]

The title compound H2(C4H10N2)](SO4)(H2O) (C4H14N2O5S) was synthesized by the reaction of MnSO4H2O with piperazine in H2O/CH3OH solution, and characterized by single-crystal X-ray diffraction analysis with the following crystal data: monoclinic, space group P21/n, a = 6.386(1), b = 11.695(2), c = 11.680(2) ? = 101.06(3)? V = 856.1(3) 3, Z = 4, Mr = 202.23 , Dc = 1.569 g/cm3, F(000) = 432 and = 0.368 mm-1. The compound consists of H2(C4H10N2)]2+, SO42- and H2O. In the structure, H2(C4H10N2)]2+ shows two kinds of chair conformations: one connects with four SO42- and two H2O molecules, and the other connects with six SO42- anions. They are arranged alternately along the b and c directions, respectively, and linked through SO42- into 2-D layers which are stacked along the a direction by NH…O, CH…O and OH…O hydrogen bonds, leading to a 3-D supramolecular compound. TGA studies indicate that the compound is thermally stable below 92 ℃.