Abstract
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 NameAffiliation
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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