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〔Mn2(TNR)2(CHZ)2(H2O)4〕·2H2O的合成和晶体结构

Preparation and Crystal Structure of 〔Mn2(TNR)2(CHZ)2(H2O)4〕·2H2O

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【作者】 张同来吕春华乔小晶蔡瑞娇郁开北

【Author】 ZHANG Tong Lai * LU Chun Hua QIAO Xiao Jing CAI Rui Jiao (Department of Mechano electric Engineering, Beijing Institute of Technology, Beijing 100081) YU Kai Bei (Chengdu Branch of Academia Sinica, Chengdu 610041)

【机构】 北京理工大学机电工程系!北京100081中科院成都分院!成都640041

【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。

【Abstract】 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.\;

  • 【文献出处】 结构化学 ,CHINESE JOURNAL OF STRUCTUNAL CHEMISTRY , 编辑部邮箱 ,1999年06期
  • 【分类号】O641.4
  • 【被引频次】18
  • 【下载频次】133
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