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Synthesis and Crystal Structure of a Ternary Complex: [Ni(phen)_2(pmal)]·8H_2O

机译:[Ni(phen)_2(pmal)]·8H_2O三元配合物的合成和晶体结构

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摘要

A new ternary complex [Ni(phen)(pmal)]·8H_2O (phen = 1,10-phenanthroline, pmal~(2-) = phenethyl malonic acid) has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex: triclinic system, space group P1, a = 10.387(5), b = 13.112(6), c = 14.229(6) A, α = 76.176(7), β = 83.778(8), γ = 71.770(6)°, C_(35)H_(42)N_4O_(12)Ni, M_r = 769.44, Z = 2, F(000) = 808, V = 1786.1 A~3, D_c = 1.431 g/cm~3, μ = 0.612 mm~(-1), the final R = 0.0653 and wR = 0.1033 for 9379 (R_(int) = 0.0244) independent reflections and 4730 observed reflections (I > 2σ(I)). Structural analysis shows that the coordination geometry of Ni(Ⅱ) is a distorted octahedron. A novel two-dimensional structure is constructed from (H_2O)_4 and (H_2O)_(12) water clusters, and the complex forms a 3-D network supramolecular structure by hydrogen bonds and π-π stacking of neighboring phens.
机译:通过乙酸镍,苯酚和苯乙基丙二酸的反应合成了一种新的三元络合物[Ni(phen)(pmal)]·8H_2O(phen = 1,10-菲咯啉,pmal〜(2-)=苯乙基丙二酸)。 。进行元素分析,IR光谱和X射线单晶衍射以确定组成和晶体结构。该复合物的晶体数据:三斜晶系,空间群P1,a = 10.387(5),b = 13.112(6),c = 14.229(6)A,α= 76.176(7),β= 83.778(8),γ = 71.770(6)°,C_(35)H_(42)N_4O_(12)Ni,M_r = 769.44,Z = 2,F(000)= 808,V = 1786.1 A〜3,D_c = 1.431 g / cm〜 3,μ= 0.612 mm〜(-1),对于9379(R_(int)= 0.0244)独立反射和4730观察到的反射(I>2σ(I)),最终R = 0.0653和wR = 0.1033。结构分析表明,Ni(Ⅱ)的配位几何是畸变的八面体。由(H_2O)_4和(H_2O)_(12)水团簇构建了一种新颖的二维结构,该复合物通过氢键和相邻phen的π-π堆积形成了3-D网络超分子结构。

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