Crystal structures of complexes between alkali-metal salts and cyclic polyethers. Part I. Complex formed between rubidium sodium isothiocyanate and 2,3,11,12-dibenzo-1,4,7,10,13,16-hexaoxocyclo-octadeca-2,11-diene (‘dibenzo-18-crown-6’)
Crystal structures of complexes between alkali-metal salts and cyclic polyethers. Part I. Complex formed between rubidium sodium isothiocyanate and 2,3,11,12-dibenzo-1,4,7,10,13,16-hexaoxocyclo-octadeca-2,11-diene (‘dibenzo-18-crown-6’)
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碱金属盐和环状聚醚之间的配合物的晶体结构第一部分：异硫氰酸钠铷钠和2,3,11,12-二苯并-1,4,7,10,13,16-六氧环-十八烷-2之间形成的配合物。 ,11-二烯（二苯并-18-冠-6）
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发表时间：
1970
期刊：
影响因子：
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通讯作者：
M. Truter
中科院分区：
文献类型：
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作者：
D. Bright;M. Truter
用三维X射线单晶衍射法测定了2，3，11，12-二苯并-1，4，7，10，13，16-六氧代环十八碳-2，11-二烯（简称“二苯并-18-冠-6”）与异硫氰酸铷钠形成的配合物的晶体结构，确定了配合物的化学式[（Rb 0·55，Na 0·45）NCS（C20 H24 O 6）]。该晶体还含有二苯并-18-冠-6的未络合分子，其具有与络合分子相同的键长和键角，但构象不同。单斜晶胞中有四个配合物分子和两个中心对称的未配合醚分子，晶胞参数为a= 19·322，B= 12·948，c= 13·001 A，β= 105·78°，空间群为P21/a。通过直接方法，然后通过傅立叶和差分傅立叶合成来解决结构。全矩阵精修法的收敛值为R 0·116，络合醚中的6个氧原子与金属原子共面且距离相等，Rb-O（平均）为2·91，Na-O（平均）为2·80.铷的六方金字塔由异硫氰酸根的氮（Rb-N 2·91 A）完成，但钠不与阴离子（Na-N 3·32 A）接触。
A three-dimensional X-ray crystal structure analysis has been carried out on a complex formed from 2,3,11,12-dibenzo-1,4,7,10,13,16-hexaoxocyclo-octadeca-2,11-diene (known as ‘dibenzo-18-crown-6’) and rubidium sodium isothiocyanate and the chemical formula [(Rb0·55, Na0·45)NCS(C20H24O6)] established. The crystal also contains uncomplexed molecules of dibenzo-18-crown-6 which have the same bond lengths and angles as, but a different conformation from, the complexed molecules. There are four molecules of complex and two centro-symmetrical molecules of uncomplexed ether in a monoclinic unit cell having a= 19·322, b= 12·948, c= 13·001 A, β= 105·78°, and space group P21/a. The structure was solved by direct methods, followed by Fourier and difference Fourier syntheses. All the atoms including hydrogen have been located; full-matrix refinement converged with R 0·116.The six oxygen atoms of the complexed ether are coplanar and equidistant from the metal atom, with Rb–O(mean) 2·91 and Na–O(mean) 2·80 A. A hexagonal pyramid about the rubidium is completed by the nitrogen of the isothiocyanate (Rb-N 2·91 A) but the sodium is not in contact with the anion (Na-N 3·32 A).