摘要
将ＭｎＣＯ３ 与２，４，６－三硝基间苯二酚（斯蒂芬酸、ＴＮＲ）分散于蒸馏水中， 加热搅拌制备出斯蒂酚酸锰溶液，再与碳酰肼（ＣＨＺ）水溶液反应制备〔Ｍｎ２ （ＴＮＲ）２（ＣＨＺ）２（Ｈ２Ｏ）４〕·２Ｈ２Ｏ（Ｃ１４Ｈ２６Ｍｎ２Ｎ１４Ｏ２４， Ｍｒ＝ ８８４．３６），并对其进行了元素分析和红外表征，利用单晶分析测定了晶体结构。该化合物为双核配合物，属三斜晶系，空间群为Ｐ１，晶体学数据如下：ａ＝ ７．２８０（１），ｂ＝ １０．３１８（１），ｃ＝ １１．１０６（１），α＝ ９４．５６（１），β＝ ９１．８６（１），γ＝ １０６．８８（１）°，Ｖ＝ ７９４．４（２）３，Ｚ＝ １，Ｄｃ＝ １．８４９ｇ．ｃｍ － ３， μ＝９．１５ｃｍ － １， Ｆ（０００）＝ ４５０， Ｉ＞ ２σ（Ｉ）的独立可观测点个数为２７８３，最终偏离因子Ｒ＝０．０２７２， Ｒｗ ＝ ０．０６３９。分子为中心对称，配位多面体为略有畸变的五角双锥体构型。
The coordination compound of 〔Mn 2(TNR) 2(CHZ) 2(H 2O) 4〕·2H 2O was prepared by mixing carbohydrazide solution and manganese styphnate solution of which was obtained through the reaction of manganese carbonate and styphnic acid. The title compound was characterized by using element analysis and FTIR. The crystal structure of 〔Mn 2(TNR) 2(CHZ) 2(H 2O) 4〕·2H 2O (C 14 H 26 Mn 2N 14 O 24 , M r =884.36) was determined by using single crystal diffraction. The crystalline was triclinic with space group \$P\$1. The unit cell parameters were as follows: a=7.280(1), b=10.318(1), c=11.1060(10), α=94.56(1), β=91.86(1), γ=106.88(1)°, V=794.4(2) 3, Z=1, D c =1.849g·cm -3 , μ =9.15cm -1 , F (000)=450. The final R =0.0272 and wR =0.0639 for 2783 observed independent reflections. The molecule existed as a central symmetry with a distorted pentagonal bipyramid configuration.\;
关键词
锰配合物
斯蒂芬酸锰
碳酰肼
合成
晶体结构
manganese styphnate,carbohydrazide, preparation,crystal structure
