2,2'-联吡啶-6,6'-二甲酸镍(Ⅱ)配合物的合成与表征

人工晶体学报 ›› 2021, Vol. 50 ›› Issue (8): 1452-1456.

2,2'-联吡啶-6,6'-二甲酸镍(Ⅱ)配合物的合成与表征

谭思慧, 刘婷, 钟国清

西南科技大学材料科学与工程学院,绵阳 621010

收稿日期:2021-04-16 出版日期:2021-08-15 发布日期:2021-09-14
通讯作者: 钟国清,教授。E-mail:zgq316@163.com
作者简介:谭思慧(1998—),女,四川省人,硕士研究生。E-mail:1434196199@qq.com
基金资助:
西南科技大学龙山学术人才科研支持计划(17LZX414)

Synthesis and Characterization of Ni(Ⅱ) Complex of 2,2'-Bipyridine-6,6'-Dicarboxylic Acid

TAN Sihui, LIU Ting, ZHONG Guoqing

School of Material Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, China

Received:2021-04-16 Online:2021-08-15 Published:2021-09-14

摘要/Abstract

摘要： 以2,2'-联吡啶-6,6'-二甲酸(6,6'-H₂bpdc)和乙酸镍为原料,用水热法合成配合物[Ni(6,6'-Hbpdc)₂]·4H₂O (1)。用元素分析、X射线粉末衍射和单晶衍射、红外光谱对配合物1的组成和结构进行了表征,并研究了其热稳定性。单晶结构显示,配合物1属于三斜晶系,P1空间群,晶胞参数为a=1.011 2(9) nm、b=1.084 9(9) nm、c=1.267 6(11) nm、α=112.672(2)°、β=101.025(3)°、γ=90.008(3)°。配合物1的中心Ni²⁺与配体中的N、O原子配位,形成六配位的扭曲八面体几何构型,并通过分子间氢键形成三维超分子结构。热稳定性研究表明,配合物1在氮气气氛中的热分解反应包括脱水和配体的氧化分解,最后残余物为NiO。

关键词: 2,2'-联吡啶-6,6'-二甲酸, 镍(Ⅱ)配合物, 水热法, 晶体结构, 热稳定性

Abstract: The complex [Ni(6,6'-Hbpdc)₂]·4H₂O (1) was synthesized with 2,2'-bipyridine-6,6'-dicarboxylic acid (6,6'-H₂bpdc) and nickel acetate as main raw materials by hydrothermal method. The composition and structure were characterized by elemental analyses, X-ray powder diffraction and single crystal diffraction, FT-IR spectra, and its thermal stability was also studied. The structure analyses show that the complex 1 is triclinic with space groups of P1. The cell parameters are a=1.011 2(9) nm, b=1.084 9(9) nm, c=1.267 6(11) nm, α=112.672(2)°, β=101.025(3)° and γ=90.008(3)°. The central nickel ion is coordinated by oxygen and nitrogen atoms in the ligand to form a distorted octahedral configuration with the coordination number of six, and the complex 1 forms a three-dimensional supramolecular structure through weak hydrogen bonds between molecules. The thermal stability study shows that the thermal decomposition reaction of complex 1 in nitrogen atmosphere include dehydration and oxidation decomposition of the ligand and the final residue is NiO.

Key words: 2,2'-bipyridine-6,6'-dicarboxylic acid, nickel(Ⅱ) complex, hydrothermal method, crystal structure, thermal stability

中图分类号:

O641.4

谭思慧, 刘婷, 钟国清. 2,2'-联吡啶-6,6'-二甲酸镍(Ⅱ)配合物的合成与表征[J]. 人工晶体学报, 2021, 50(8): 1452-1456.

TAN Sihui, LIU Ting, ZHONG Guoqing. Synthesis and Characterization of Ni(Ⅱ) Complex of 2,2'-Bipyridine-6,6'-Dicarboxylic Acid[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2021, 50(8): 1452-1456.

参考文献

[1] REN Y L, WANG F, HU H M, et al. Lanthanide coordination compounds with 2, 2'-bipyridine-6, 6'-dicarboxylate: synthesis, crystal structure, luminescence and magnetic property[J]. Inorganica Chimica Acta, 2015, 434: 104-112.
[2] OU Y C, ZHONG J X, SONG Y Y, et al. Two 1D chain structures derived from alkaline-earth metal complexes and 2, 2'-bipyridine-5, 5'-dicarboxylate ligand: syntheses, crystal structures and luminescent properties[J]. Chinese Journal of Inorganic Chemistry, 2016, 32(4): 738-744.
[3] 黄妙龄,杨一泓,骆杰烽,等.配合物2[NiL₂(H₂O)₂]·DMF的合成、晶体结构与荧光性质的研究[J].人工晶体学报,2020,49(2):276-280+285.
HUANG M L, YANG Y H, LUO J F, et al. Synthesis, crystal structure and fluorescent properties of the complex 2[NiL₂(H₂O)₂]·DMF[J]. Journal of Synthetic Crystals, 2020, 49(2): 276-280+285(in Chinese).
[4] ZHANG L, JIANG C, GUO L F, et al. Synthesis, characterization, antitumor activity, and theoretical calculations of Co(Ⅱ) complex based on pyridine-2, 6-dicarboxylic acid[J]. Chinese Journal of Inorganic Chemistry, 2021, 37(2): 368-374.
[5] LIU Z, GAO Y, YU Z, et al. Effects of Br substituent on catalytic performance of Ru-bda (H₂bda=2, 2'-bipyridine-6, 6'-dicarboxylic acid) catalysts for water oxidation[J]. Chinese Journal of Catalysis, 2015, 36(10): 1742-1749.
[6] TSHUMA P, MAKHUBELA B C E, NDAMYABERA C A, et al. Synthesis and characterization of 2D metal-organic frameworks for adsorption of carbon dioxide and hydrogen[J]. Frontiers in Chemistry, 2020, 8: 581226.
[7] LI R F, LI R H, LIU X F, et al. Correction: lanthanide complexes based on a conjugated pyridine carboxylate ligand: structures, luminescence and magnetic properties[J]. RSC Advances, 2020, 10(14): 8539.
[8] RÖNFELDT P, RUSER N, REINSCH H, et al. New scandium-containing coordination polymers with linear linker molecules: crystal structures and luminescence properties[J]. European Journal of Inorganic Chemistry, 2020, 2020(28): 2737-2743.
[9] LI C, YUE Q, XU Y, et al. 3-D lanthanide-organic frameworks constructed by 2, 2'-bipyridine-3, 3'-dicarboxylic acid and oxalic acid: structure, photoluminescence and luminescent sensing properties[J]. Journal of Molecular Structure, 2020, 1209: 127947.
[10] YAO L Y, YANG F, LIANG W B, et al. Ruthenium complex doped metal-organic nanoplate with high electrochemiluminescent intensity and stability for ultrasensitive assay of mucin 1[J]. Sensors and Actuators B: Chemical, 2019, 292: 105-110.
[11] XIE J H, ZHENG B C, LI B. Synthesis, crystal structures and characterization of iron(Ⅲ) and cobalt(Ⅲ) complexes bearing 2, 2'-bipyridylcarboxylate ligands[J]. Transition Metal Chemistry, 2019, 44(5): 425-430.
[12] ZHONG G Q, ZHONG Q. Solid-solid synthesis, characterization, thermal decomposition and antibacterial activities of zinc(Ⅱ) and nickel(Ⅱ) complexes of glycine-vanillin Schiff base ligand[J]. Green Chemistry Letters and Reviews, 2014, 7(3): 236-242.
[13] 李迪,顾梅,钟国清.乙二胺四乙酸铋(Ⅲ)双核配合物的合成和晶体结构[J].人工晶体学报,2013,42(12):2726-2731.
LI D, GU M, ZHONG G Q. Synthesis and crystal structure of dinuclear bismuth(Ⅲ) complex with ethylenediaminetetraacetate[J]. Journal of Synthetic Crystals, 2013, 42(12): 2726-2731(in Chinese).
[14] LUO H, YANG R G, CHEN Z H, et al. A novel homodinuclear ternary coordination polymer of nickel(Ⅱ) based on two rigid ligands: solvothermal synthesis, crystal structure, luminescent and magnetic properties[J]. Journal of Solid State Chemistry, 2020, 291: 121587.
[15] TAHA Z A, HIJAZI A K. Structural and photophysical properties of lanthanide complexes with N'-(2-methoxybenzylidene)-2-pyridinecarbohydrazide Schiff base ligand: catalyzed oxidation of anilines with hydrogen peroxide[J]. Journal of Molecular Structure, 2021, 1238: 130451.