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双-[μ-,双-(2-氨基乙基)乙烷-1,2-二胺]-双-[,双-(2-氨基乙基)乙烷-1,2-二胺]-μ-氧代-六-μ-氧代-八-μ-氧代-四-氧化四镍(II)六钽(V)十九水合物的合成与晶体结构

Synthesis and crystal structure of bis-[μ-,-bis-(2-amino-eth-yl)ethane-1,2-di-amine]-bis-[,-bis-(2-amino-eth-yl)ethane-1,2-di-amine]-μ-oxido-hexa-μ-oxido-octa-μ-oxido-tetra-oxido-tetra-nickel(II)hexa-tantalum(V) nona-deca-hydrate.

作者信息

Krause Dana-Céline, Näther Christian, Bensch Wolfgang

机构信息

Institut für Anorganische Chemie, Christian-Albrechts-Universität zu Kiel, Max-Eyth-Str. 2, D-24118 Kiel, Germany.

出版信息

Acta Crystallogr E Crystallogr Commun. 2021 Nov 9;77(Pt 12):1253-1257. doi: 10.1107/S2056989021011531. eCollection 2021 Dec 1.

Abstract

Reaction of K{TaO}·16HO with [Ni(tren)(HO)Cl]Cl·HO in different solvents led to the formation of single crystals of the title compound, [NiTaO(CHN)]·19HO or {[Ni(κ-tren)(μ-κ-tren)]TaO}·19HO (tren is ,-bis-(2-amino-eth-yl)-1,2-ethanediamine, CHN). In its crystal structure, one Lindqvist-type anion {TaO} (point group symmetry ) is connected to two Ni cations, with both of them coordinated by one tren ligand into discrete units. Both Ni cations are sixfold coordinated by O atoms of the anion and N atoms of the organic ligand, resulting in slightly distorted [NiON] octa-hedra for one and [NiON] octa-hedra for the other cation. These clusters are linked by inter-molecular O-H⋯O and N-H⋯O hydrogen bonding involving water mol-ecules into layers parallel to the plane. Some of these water mol-ecules are positionally disordered and were refined using a split model. Powder X-ray diffraction revealed that a pure crystalline phase was obtained but that on storage at room-temperature this compound decomposed because of the loss of crystal water mol-ecules.

摘要

K{TaO}·16H₂O与[Ni(tren)(H₂O)Cl]Cl·H₂O在不同溶剂中反应,生成了标题化合物[NiTaO(CH₆N₃)]·19H₂O或{[Ni(κ-tren)(μ-κ-tren)]TaO}·19H₂O(tren为N,N,N',N'-四(2-氨基乙基)-1,2-乙二胺,CH₆N₃)的单晶。在其晶体结构中,一个Lindqvist型阴离子{TaO}(点群对称性 )与两个Ni阳离子相连,二者均由一个tren配体配位形成离散单元。两个Ni阳离子均由阴离子的O原子和有机配体的N原子六配位,导致其中一个阳离子形成略微扭曲的[NiO₆N₂]八面体,另一个阳离子形成[NiO₅N₃]八面体。这些簇通过涉及水分子的分子间O-H⋯O和N-H⋯O氢键连接成平行于 平面的层。其中一些水分子位置无序,采用分裂模型进行精修。粉末X射线衍射表明得到了纯晶相,但该化合物在室温下储存时因结晶水分子的损失而分解。

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