Synthesis of 1,2,4,5-Benzenetetrasulfonic Acid (H4B4S) and its Implementation as a Linker for Building Metal-Organic Frameworks on the Example of [Cu2(B4S)(H2O)8]·0.5H2O

Synthesis of 1,2,4,5-Benzenetetrasulfonic Acid (H4B4S) and its Implementation as a Linker for Building Metal-Organic Frameworks on the Example of [Cu2(B4S)(H2O)8]·0.5H2O
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以[Cu2(B4S)(H2O)8]·0.5H2O为例,1,2,4,5-苯四磺酸(H4B4S)的合成及其作为构建金属有机骨架连接体的应用

DOI:
10.1002/zaac.201000056
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发表时间:
2010
期刊:
Zeitschrift für anorganische und allgemeine Chemie
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--
通讯作者:
M. Wickleder
M. Wickleder
中科院分区:
--
文献类型:
--
作者:
Thomas W. T. Muesmann;Andrea Mietrach;J. Christoffers;M. Wickleder

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从1,2,4,5-四氯苯开始,以两个步骤制备苯1,2,4,5-四磺酸(H4 B4 S)。H4 B4 S和Cu 2(OH)2(CO 3)的含水反应混合物的缓慢蒸发导致[Cu 2(B4 S)(H2O)8] · 0.5 H2O的浅绿色单晶。X-射线单晶结构分析表明该化合物为三斜晶系[P-1,Z = 1,a = 710.0(1),B = 713.7(1),c = 1077.1(2)pm,α = 98.41(2)°,β = 102.91(2)°,γ = 100.69(2)°]。在晶体结构中,Cu 2+离子被四个水分子和两个单齿磺酸根阴离子配位,产生四方扭曲的[CuO 6]八面体。阴离子与铜离子连接,形成沿[110]方向沿着延伸的梯形链。根据DTA/TG研究,化合物的脱水在240°C完成,无水磺酸盐的分解在340°C开始。
Benzene 1,2,4,5-tetrasulfonic acid (H4B4S) was prepared in two steps starting from 1,2,4,5-Te¬tra¬chlorobenzene. Slow evaporation of an aqueous reaction mixture of H4B4S and Cu2(OH)2(CO3) led to light green single crystals of [Cu2(B4S)(H2O)8] • 0.5 H2O. X-ray single crystal investi¬ga¬tions revealed the compound to be triclinic [P-1, Z = 1, a = 710.0(1), b = 713.7(1), c = 1077.1(2) pm, α = 98.41(2)°, β = 102.91(2)°, γ = 100.69(2)°]. In the crystal struc-ture the Cu2+ ions are coordinated by four water molecules and two monodentate sulfo¬na¬te anions yielding a tetragonally distorted [CuO6] octahedron. The anions are connected to fur-ther copper ions leading to ladder shaped chains running along the [110] direction. Accor¬ding to DTA/TG investi¬gations the dehydration of the compound is finished at 240°C and the de-com¬position of the anhydrous sulfonate starts at 340°C.