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Solid-Solid Synthesis, Crystal Structure and Thermal Decomposition of Copper(II) Complex of 2-Picolinic Acid

机译:2-吡啶甲酸铜(II)配合物的固溶合成,晶体结构和热分解

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摘要

The copper(II) complex [Cu(pic)(2)]center dot 2H(2)O was synthesized with 2-picolinic acid (Hpic) and copper acetate as reactants by room temperature solid-solid reaction. The composition and structure of the complex was characterized by elemental analyses, single crystal X-ray diffraction, X-ray powder diffraction, FT-IR spectroscopy and thermogravimetry-differential scanning calorimetry. The crystal structure of the copper(II) complex belongs to triclinic system and space group, with cell parameters of a = 5.1274(16) angstrom, b = 7.641(2) angstrom, c = 9.209(2) angstrom, a = 74.91(2)degrees, beta = 84.56(2)degrees, gamma = 71.58(3)degrees, V = 338.48(15) angstrom(3), Z = 1, F(000) = 175, R-1 = 0.0530, and wR(2) = 0.1141. The Cu(II) ion is six-coordinated through two nitrogen atoms from two pyridine rings and four carboxyl oxygen atoms from four different 2-picolinic acid anions, forming an elongated octahedral geometry. The interaction of carboxylate O and Cu(II) forms an one-dimensional chain structure, and the complex exhibits a two-dimensional layered structure by hydrogen bonds. The thermal decomposition processes of the complex under air include dehydration and pyrolysis of the ligand, and the final residue at about 400 degrees C is copper oxide.
机译:以2-吡啶甲酸(Hpic)和乙酸铜为反应物,通过室温固-固反应合成了铜(II)配合物[Cu(pic)(2)]中心点2H(2)O。通过元素分析,单晶X射线衍射,X射线粉末衍射,FT-IR光谱和热重分析-差示扫描量热法对复合物的组成和结构进行了表征。铜(II)配合物的晶体结构属于三斜晶系和空间群,单元参数为a = 5.1274(16)埃,b = 7.641(2)埃,c = 9.209(2)埃,a = 74.91( 2)度,beta = 84.56(2)度,γ= 71.58(3)度,V = 338.48(15)埃(3),Z = 1,F(000)= 175,R-1 = 0.0530,和wR (2)= 0.1141。 Cu(II)离子通过来自两个吡啶环的两个氮原子和来自四个不同的2-吡啶甲酸阴离子的四个羧基氧原子进行六配位,形成细长的八面体几何形状。羧酸盐O和Cu(II)的相互作用形成一维链结构,并且该配合物通过氢键呈现二维分层结构。络合物在空气中的热分解过程包括配体的脱水和热解,最终的残留物在约400摄氏度时为氧化铜。

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