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铟-水杨酰羟肟酸络合阳离子的晶体结构:[In(Hshi)(HO)](NO)·8.57HO

Crystal structure of an indium-salicyl-hydroximate complex cation: [In(Hshi)(HO)](NO)·8.57HO.

作者信息

Aziz Ozha A, Zeller Matthias, Zaleski Curtis M

机构信息

Department of Chemistry and Biochemistry, Shippensburg University, Shippensburg, PA 17257, USA.

Department of Chemistry, Purdue University, West Lafayette, IN 47907, USA.

出版信息

Acta Crystallogr E Crystallogr Commun. 2022 Aug 18;78(Pt 9):926-931. doi: 10.1107/S2056989022007964. eCollection 2022 Sep 1.

Abstract

The synthesis and crystal structure for the title compound, hexa-aqua-hexa-kis(μ-2-hy-droxy-benzene-carbo-hydrox-a-mato)bis-(2-hy-droxy-benzene-carbo-hydrox-a-m-ato)tetra-indium(III) tetra-nitrate 8.57-hydrate + unknown solvent, In(Hshi)(HO)·8.57HO·solvent, where Hshi is salicylhydrox-imate (CHNO), are reported. The complex cation of the structure, [In(Hshi)(HO)], is a dimer with a step-like topology and possesses an inversion center that relates each [In(Hshi)(HO)] side of the complex cation. Each In ion is seven-coordinate with a penta-gonal-bipyramidal geometry, and the salicyl-hydroximate ligands have a 1- charge as only the oxime oxygen of the ligand is deprotonated. Four inter-stitial nitrate anions maintain the charge balance of the compound. One of the nitrate anions (and its symmetry equivalent) is disordered over two different orientations with an occupancy ratio of 0.557 (7) to 0.443 (7). The inter-stitial solvent water mol-ecules show substantial disorder. Approximately 8.57 water mol-ecules per formula unit were refined as disordered and partially occupied, while a suitable model could not be devised for the other extensively disordered solvent mol-ecules (water and possibly methanol as this was the synthesis solvent). Thus, these latter solvent mol-ecules were instead treated with the SQUEEZE routine [Spek (2015). . C, 9-18.] as implemented in the program , and the procedure corrected for 151 electrons within solvent-accessible voids of 367 Å.

摘要

报道了标题化合物六水合六(μ-2-羟基苯甲酰羟胺基)双(2-羟基苯甲酰羟胺基)四铟(III)四硝酸盐8.57水合物+未知溶剂,即In(Hshi)(H₂O)₆₄·8.57H₂O·溶剂,其中Hshi为水杨酰羟肟酸(C₇H₇NO₃)。该结构的络合阳离子[In(Hshi)(H₂O)₆]是具有阶梯状拓扑结构的二聚体,且具有一个对称中心,该对称中心关联着络合阳离子的每个[In(Hshi)(H₂O)₆]面。每个In离子为七配位,呈五角双锥几何构型,水杨酰羟肟酸配体带1-电荷,因为只有配体的肟氧去质子化。四个间隙硝酸根阴离子维持化合物的电荷平衡。其中一个硝酸根阴离子(及其对称等效物)在两个不同取向上无序分布,占有率为0.557 (7) 至0.443 (7)。间隙溶剂水分子表现出显著的无序性。每分子式单元约8.57个水分子被精修为无序且部分占据,而对于其他广泛无序的溶剂分子(水以及可能的甲醇,因为这是合成溶剂)无法设计出合适的模型。因此,这些后一种溶剂分子改用程序中实施的SQUEEZE程序[Spek (2015). Acta Cryst. C, 9-18.]处理,该程序校正了367 Å溶剂可及空隙内的151个电子。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3366/9443793/08e586fbd835/e-78-00926-fig1.jpg

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