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四(亚硝基)合钯酸钾的合成、单晶结构及其循环伏安特征 |
Synthesis, single-crystal structure and cyclic voltammetry of potassium tetranitropalladate(II) |
Received:November 03, 2022 |
DOI: |
中文关键词: 结构化学 四亚硝基钯酸钾(K2[Pd(NO2)4]) 合成 晶体结构 循环伏安 |
英文关键词: structural chemistry potassium tetranitropalladate(II) (K2[Pd(NO2)4]) synthesis crystal structure cyclic voltammetry |
基金项目:云南省基础研究计划面上项目(202001AT070090);云南省技术创新人才项目(202305AD160019);云南省省市一体化专项(202302AH360001);云南省院所技术开发专项(202104AR040016);云南省重大科技专项(202102AB080007);云南贵金属实验室科技计划项目(YPML-2022050231) |
Author Name | Affiliation | GAO Anli | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | GUO Xuhu | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | ZHANG Ke | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | CHEN Zhuan | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | TANG Ling | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | YU Juan | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China | LIU Jun | State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Kunming Institute of Precious Metals, Kunming 650106, China |
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中文摘要: |
以醋酸钯(PdAc2)与亚硝酸钾(KNO2)为起始原料,水为溶剂,合成四亚硝基钯酸钾(K2[Pd(NO2)4]),产率为96.5%。采用溶剂挥发法培养出其单晶,经X射线单晶衍射分析证实:此晶体由中心对称的[Pd(NO2)4]2-配阴离子,K+阳离子和2分子结晶水组成,为三斜晶系,P-1空间群,晶胞参数为:a=6.4953(5) nm,b=7.0134(5) nm,c=7.1473(5) nm,α=118.784(2)°,β=101.050(2)°,γ=98.085(2)°,Z=1,Pd-N键长为2.014 nm和2.037 nm,∠N-Pd-N为91.70(4)°,且Pd2+位于4个N原子组成的平面四边形的中心。采用恒电位仪在室温下测试其循环伏安图,测得其还原峰电位(Ep)为-0.51 V (vs. SCE)。 |
英文摘要: |
Potassium tetranitropalladate(II) was synthesized in one step by mixing palladium acetate and potassium nitrite in water with a yield of 96.5%. A single crystal of the product was cultivated using a solvent evaporation method, and was characterized by X-ray single crystal diffraction analysis. The crystal unit of the compound contains one centrosymmetric [Pd(NO2)4]2- complex anion, two K+ cations and two crystallized water molecules, belongs to triclinic crystal system and P-1 space group. The unit cell parameters are a=6.4953(5) nm, b=7.0134(5) nm, c=7.1473(5) nm, α=118.784(2)°, β=101.050(2)°, γ=98.085(2)°, Z=1. The Pd-N bond lengths are 2.014 and 2.037 nm, ∠N-Pd-N is 91.70(4)°, revealing that Pd2+ is in the center of the planar quadrilateral formed by four N atoms from the nitro groups. The cyclic voltammetry was measured at room temperature, and the reduction peak potential (Ep) was found to be -0.51 V (vs. SCE). |
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