Synthesis, Crystal Structure and Hirshfeld Surface Analysis of Bis(Benzene-1,2-Diamie)-Bis(2,4-Dihidroxybenzoato)-Nickel, [Ni(C6H8N2)2(C7H5O4)2]

IF 0.4 4区化学 Q4 CRYSTALLOGRAPHY

Journal of Chemical Crystallography Pub Date : 2025-04-10 DOI:10.1007/s10870-025-01046-5

Abdukadir Kh. Tashkulov, Khayit Kh. Turaev, Jamshid M. Ashurov, Ahatov Alisher Ashur o’g’li, Bekmurod A. Khurramovich, Aziz B. Ibragimov, Changkun Xia, Abul Monsur Showkot Hossain

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引用次数: 0

Abstract

The title compound, [Ni(C₆H₈N₂)₂(C₇H₅O₄)₂] was obtained by dissolving of o-phenylenediamine (OPDA), nickel (II) sulfate and 2,4-dihydroxybenzoic acid (2,4-DHB) separately in 10 mL of ethanol (96%) and reacting with 10 mL of distilled water. The reaction mixture was stirred at room temperature and then slowly evaporated the pale green solution at 55–60 °C. The composition and crystal structure of the [Ni(C₆H₈N₂)₂(C₇H₅O₄)₂], complex was obtained at a constant temperature (30 ± 1 ºC) in 12 days. The complex is formed with two neutral bidentate OPDA ligands and two monodentate DHB ligands as [Ni(C₆H₈N₂)₂(C₇H₅O₄)₂]. The Ni atom is located at the inversion center, exhibiting a slightly octahedrally distorted coordination environment, with four nitrogen atoms of two o -phenylenediamine ligands (Ni–N) positioned in the equatorial plane and two oxygen atoms of 2,4-dihydroxybenzoic acid located in the axial plane. Here, two Ni–N bonds [Ni1 —N1 = 2.110(3), Ni1 —N1 ⁱ = 2.110(3) are exhibited the same bond length but opposite Ni–N bands are different Ni2 —N2 = 2.131(2), Ni2 —N2 ⁱ = 2.131(2)] and a longer axial two Ni—O bonds [2.136(2)]. The metal is located around the inversion center and is almost coplanar with the NiN₄ plane. In the crystal, inter-molecular hydrogen bonding interactions are observed at N1— H1..O1 and N2 — H2…O1 in the periodic network structure. The Hirshfeld surface analysis report indicates that the most important contributions to the crystal packing are H…H (44.6%), H….C/C….H (28.7%), O…H/H….O (23.7%), O…C/C….O (2.5%), C…C (1.7%), O…O(0.8%) interactions.

Graphical Abstract

The paper is designed by crystal structures of Ni(II) complex containing [Ni(C₆H₈N₂)₂(C₇H₅O₄)₂]. In continuation of our interest in the combination forms of benzene-1,2-diamine (ortho-phenylenediamine = OPDA) and 2,4-dihydroxybenzoic acid (2,4-DHB) with first-line conversion of metals, the authors considered a detailed discussion of the structure analysis of the Ni(II) complex from the mixed ligand of OPDA and 2,4-DHB using X-ray crystallographic technique

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双（苯-1,2-二胺）-双（2,4-二羟苯甲酸酯）-镍，[Ni(C6H8N2)2(C7H5O4)2]的合成、晶体结构和Hirshfeld表面分析

将邻苯二胺（OPDA）、硫酸镍（II）和2,4-二羟基苯甲酸（2,4- dhb）分别溶解于10 mL（96%）乙醇中，与10 mL蒸馏水反应，得到标题化合物[Ni(C6H8N2)2(C7H5O4)2]。将反应混合物在室温下搅拌，然后在55-60℃下缓慢蒸发淡绿色溶液。在恒温（30±1℃）条件下，用12天的时间得到了[Ni(C6H8N2)2(C7H5O4)2]配合物的组成和晶体结构。该配合物由两个中性双齿OPDA配体和两个单齿DHB配体组成[Ni(C6H8N2)2(C7H5O4)2]。Ni原子位于反转中心，呈现出轻微的八面体畸变配位环境，两个邻苯二胺配体（Ni - n）的4个氮原子位于赤道面，2,4-二羟基苯甲酸的2个氧原子位于轴向面。在这里，两个Ni-N键[Ni1 -N1 = 2.110(3), Ni1 -N1 i = 2.110(3)]具有相同的键长，但相反的Ni-N带不同：Ni2 -N2 = 2.131(2), Ni2 -N2 i = 2.131(2)]和一个更长的轴向两个Ni-O键[2.136(2)]。金属位于反转中心周围，几乎与NiN4平面共面。在晶体中，分子间的氢键相互作用在N1 - H1上被观察到。O1和N2 - H2…O1在周期性网络结构中。Hirshfeld表面分析报告表明，对晶体堆积最重要的贡献是H…H (44.6%)， H....C/C....H (28.7%), O…H/H....O (23.7%), O…c / c ....O(2.5%), C…C (1.7%), O…O（0.8%）相互作用。本文采用含[Ni(C6H8N2)2(C7H5O4)2]的Ni（II）配合物的晶体结构进行设计。为了继续我们对苯-1,2-二胺（邻苯二胺= OPDA）和2,4-二羟基苯甲酸（2,4- dhb）的结合形式与一线金属转化的兴趣，作者考虑使用x射线晶体学技术对OPDA和2,4- dhb混合配体的Ni（II）配合物的结构分析进行详细的讨论

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来源期刊

Journal of Chemical Crystallography 化学-光谱学

CiteScore

1.50

自引率

12.50%

发文量

审稿时长

6.3 months

期刊介绍： Journal of Chemical Crystallography is an international and interdisciplinary publication dedicated to the rapid dissemination of research results in the general areas of crystallography and spectroscopy. Timely research reports detail topics in crystal chemistry and physics and their relation to problems of molecular structure; structural studies of solids, liquids, gases, and solutions involving spectroscopic, spectrometric, X-ray, and electron and neutron diffraction; and theoretical studies.