A 2D coordination polymer assembled from a nickel(II) tetraazamacrocyclic cation and 4,40-(dimethylsilanediyl)diphthalate(3-) linker

被引：4
作者：
Gavrish S. [1 ]
Shova S. [2 ]
Cazacu M. [2 ]
Lampeka Y. [1 ]
机构：
[1] L.V. Pisarzhevskii Institute of Physical, Chemistry of the National Academy of Sciences of Ukraine, Prospekt Nauki 31, Kyiv
[2] Petru Poni Institute of Macromolecular Chemistry, Department of Inorganic Polymers, Aleea Grigore Ghica Voda 41A, Iasi
来源：
Acta Crystallographica Section C: Structural Chemistry | 2020年 / 76卷
关键词：
4; 40-(dimethylsilanediyl) diphthalic acid; crystal structure; cyclam; IR spectroscopy; nickel(II); reflection spectra; thermogravimetry; twodimensional coordination polymer;
D O I：
10.1107/S2053229620005008
中图分类号：
学科分类号：
摘要：
The preformed nickel(II) complex of the 14-membered macrocyclic ligand 1,4,8,11-tetraazacyclotetradecane (cyclam, L), when treated with 4,40-(dimethylsilanediyl) diphthalic acid (H4A) in a DMF/H2O mixture (4:1 v/v) under heating, leads to [Ni(L)]3(HA)23DMF (IDMF). Redissolution of this compound in a DMF/H2O/MeOH mixture (4:1:30 v/v/v) with mild acidification under gentle heating results in the formation of a similar compound but containing water and methanol molecules of crystallization, [Ni(L)]3(HA)25H2O2MeOH (IIH2O). At lower temperature and concentration of reactants and longer reaction time, single crystals of composition {[{Ni(L)}3(HA)2]4CH3OH}n (IIMeOH) were isolated. Single-crystal X-ray diffraction analysis of this compound, which, according to PXRD is isostructural with IIH2O but different from IDMF, revealed its two-dimensional (2D) polymeric structure, i.e. poly[[bis{3-4-[(4- carboxy-3-carboxylatophenyl)dimethylsilyl]benzene-1,2-dicarboxylato-3O1:O2:O30 }-tris(1,4,8,11-tetraazacyclotetradecane-4N)trinickel(II)] methanol tetrasolvate],{[Ni3(C18H13O8Si)2(C10H24N4)3]4CH3OH}n. It is built up of the monoprotonated tricarboxylate HA3 ligand coordinated in a monodentate manner in the axial positions of two crystallographically independent NiII cations, one of which is located on a crystallographic inversion centre. Both metal ions adopt a slightly tetragonally elongated trans-N4O2 octahedral geometry. The compound has a lamellar structure with polymeric layers oriented parallel to the (102) plane, which are in turn linked via hydrogen bonds involving protonated carboxylic acid groups of the ligand. Bulk compounds IDMF and IIH2O were characterized by FT-IR and diffuse reflectance spectroscopy and thermogravimetry, which provide evidence of their structural differences. © 2020 International Union of Crystallography.
引用
收藏
页码：419 / 426
页数：7
相关论文
共 40 条
[1]  
CrysAlis PRO, (2014)
[2]  
Barefield E.K., Wagner F., Herlinger A.W., Dahl A.R., Inorg. Synth., 16, pp. 220-224, (1976)
[3]  
Boeyens J.C.A., Dobson S.M., Stereochemistry of Organometallic and Inorganic Compounds, 2, pp. 1-83, (1987)
[4]  
Bosnich B., Poon C.K., Tobe M.C., Inorg. Chem., 4, pp. 1102-1108, (1965)
[5]  
Cazacu M., Vlad A., Zaltariov M.-F., Shova S., Novitchi G., Train C., J. Organomet. Chem., 774, pp. 70-78, (2014)
[6]  
Davies R.P., Less R., Lickiss P.D., Robertson K., White A.J.P., Cryst. Growth Des., 10, pp. 4571-4578, (2010)
[7]  
Davies R.P., Less R.J., Lickiss P.D., Robertson K., White A.J.P., Inorg. Chem., 47, pp. 9958-9964, (2008)
[8]  
Dolomanov O.V., Bourhis L.J., Gildea R.J., Howard J.A.K., Puschmann H., J. Appl. Cryst., 42, pp. 339-341, (2009)
[9]  
Farrusseng D., Metal-Organic Frameworks Applications from Catalysis to Gas Storage, (2011)
[10]  
Frahm D., Fischer M., Hoffmann F., Froba M., Inorg. Chem., 50, pp. 11055-11063, (2011)
1234