三维氢键超分子化合物[H_3cth][Fe(CN)_6]·3H_2O的合成与结构

Synthesis and Structure of a Three-dimensional Hydrogen-bonded Supramolecular Compound [H_3cth] [Fe(CN)_6]·3H_2O

用内消旋５，７，７，１２，１４，１４－六甲基－１，４，８，１１－四氮杂环十四烷（ｃｔｈ）和Ｋ_３［Ｆｅ（ＣＮ）_６〕合成了氢键连接的超分子化合物［Ｈ_３ｃｔｈ］［Ｆｅ（ＣＮ）_３］·３Ｈ_２Ｏ．该化合物的晶体属三斜晶系，Ｐ－１空间群，晶胞参数ａ＝０．９３０ ９７（９）ｎｍ，ｂ＝１．０５１ ６０（１１）ｎｍ，ｃ＝１．６３８ ４７（１７）ｎｍ，ａ＝１０１．０７７（２）°，β＝９０．８６０（２）°，γ＝１１１．６７１（２）°， Ｖ＝１．４５６ ４（３） ｎｍ３， Ｚ＝２， Ｒ＝０．０４１５．晶体中质子化的大环四胺与六氰合铁（Ⅱ ）离子之间通过氢键连接成二维层状结构，而水分子所形成的氢键使化合物呈现三维超分子网络．

A hydrogen-bonded supramolecular compound, [H3cth] [Fe(CN)6]. 3H2O, was synthesized from meso-5, 7, 7, 12, 14, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradecane (cth) and K3 [Fe (CN )6]. The compound crystallizes in triclinic space group P1, with a=0. 930 97 (9) nm, b=1. 051 60(11) nm, c=1. 638 47(17) nm, a=101. 077(2)°,β=90. 860(2)°, γ=111. 671 (2)°, V=1. 456 4(3) nm3, Z=2, R=0.0415. The structure consists of neutral two-dimensional sheets assembled via hydrogen bonds be- tween the partially protonated macrocyclic tetraamine and the hexacyanoferrate(Ⅲ) ion, while the hydrogen bonds involving water molecules interlink the sheets to form a unique three-dimensional supramolecular architecture.