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Effect of Synthesis Conditions on the Composition and Structure of Chromium(III) Complexes with Cyclobutane-1,1-Dicarboxylic Acid Anions
Russian Journal of Coordination Chemistry ( IF 1.1 ) Pub Date : 2021-02-24 , DOI: 10.1134/s1070328421020019
E. S. Bazhina , M. A. Shmelev , A. A. Korlyukov , M. A. Kiskin , I. L. Eremenko

Abstract

The reaction of Cr(NO3)3·9H2O with potassium cyclobutane-1,1-dicarboxylate (K2(Cbdc)) in 1 : 3 ratio was studied. It was shown that, depending on the reaction conditions and the solvents used for synthesis and crystallization, compounds of various compositions and structures can be isolated from the reaction system. Conducting the reaction in water followed by recrystallization from ethanol and methanol results in isolation of 2D polymeric complexes [KCr(Cbdc)2(H2O)2]n (I) and {[K4Cr2(OMe)2(Cbdc)4(MeOH)6]· MeOH}n (II), respectively. The addition of excess KOH to the same reaction mixture and recrystallization from alcohols gives rise to the crystals of 3D polymeric compound [K3Cr(Cbdc)3(H2O)2]n (III). Conducting the reaction in methanol followed by slow diffusion of diethyl ether affords complex [K3Cr(Cbdc)3(MeOH)2(H2O)2]n (IV) with a 2D polymeric structure. The crystal structures of compounds IIV were determined by X-ray diffraction (CIF files CCDC nos. 2006090 (I), 2006109 (II), 2006116 (III), and 2 006 117 (IV)).



中文翻译:

合成条件对环丁烷-1,1-二羧酸阴离子铬(III)配合物组成和结构的影响

摘要

研究了Cr(NO 33 ·9H 2 O与环丁烷-1,1-二羧酸钾(K 2(Cbdc))的比例为1:3的反应。结果表明,取决于反应条件和用于合成和结晶的溶剂,可以从反应体系中分离出各种组成和结构的化合物。在水中进行反应,然后从乙醇和甲醇中重结晶,从而分离出2D聚合物配合物[KCr(Cbdc)2(H 2 O)2 ] nI)和{[K 4 Cr 2(OMe)2(Cbdc)4(甲醇)6 ]·MeOH} nII)。向相同的反应混合物中添加过量的KOH并从醇中重结晶,生成3D高分子化合物[K 3 Cr(Cbdc)3(H 2 O)2 ] nIII)的晶体。在甲醇中进行反应,然后缓慢扩散乙醚,得到具有2D聚合结构的复合物[K 3 Cr(Cbdc)3(MeOH)2(H 2 O)2 ] nIV)。化合物IIV的晶体结构通过X射线衍射测定(CIF文件CCDC号2006090(I),2006109(II),2006116(III)和2006117 (IV))。

更新日期:2021-02-24
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