Abstract The reaction of 2-hydroxy-1-(2′-methylthiophenylazo)naphthalene (HL) with iron(II) chloride results in the formation of a hitherto unknown complex, [Fe(L) 2 ][FeCl 4 ] ( 1 ). The azo-thioether ligand binds iron(III) center through the O − ,N,S donor set to form the octahedral [Fe(L) 2 ] + cation. Solid state molecular structure of ( 1 ) has been determined by single crystal X-ray diffraction technique. Compound ( 1 ) crystallizes in the monoclinic P 2 1 / c space group of unit cell dimensions a = 10.3904(19) Å, b = 23.735(4) Å, c = 15.815(3) Å; α = 90°, β = 102.248(4)°, γ = 90° and Z = 4. The structure was solved by direct method and refined to R 1 value 0.0975 on 3796 observed reflections. There are one octahedral cationic unit of [Fe III L 2 ], a tetrahedral anionic unit of [Fe III Cl 4 ] and 0.5(C 2 H 5 OH) 2 as solvent molecules in an asymmetric unit of the crystal lattice of ( 1 ). There are two intramolecular C–H ⋯ O interactions and the crystal packing is stabilized by interionic C–H ⋯ Cl and intermolecular C–H ⋯ Cg interactions. Graphic Abstract Single crystal X-ray diffraction study of an iron(III) complex bearing an azo-thioether ligand, 2-hydroxy-1-(2′-methylthiophenylazo)naphthalene (HL) is presented, crystal packing of the complex, [Fe III L 2 ] + [Fe III Cl 4 ] − ( 1 ) has been found to be stabilized by interionic C–H ⋯ Cl and intermolecular C–H ⋯ Cg interactions.

中文翻译：

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具有 O,N,S 供体组的三齿二氮烯配体铁 (III) 配合物的合成、表征和分子结构：不对称单元中八面体和四面体铁 (III) 位点的共存

摘要 2-羟基-1-(2'-甲硫基苯基偶氮)萘 (HL) 与氯化铁 (II) 反应形成了迄今未知的络合物 [Fe(L) 2 ][FeCl 4 ] ( 1 ) . 偶氮硫醚配体通过 O - ,N,S 供体组与铁 (III) 中心结合形成八面体 [Fe(L) 2 ] + 阳离子。(1)的固态分子结构已通过单晶X射线衍射技术确定。化合物(1)在晶胞尺寸a = 10.3904(19) Å, b = 23.735(4) Å, c = 15.815(3) Å的单斜P 2 1 / c空间群中结晶；α = 90°、β = 102.248(4)°、γ = 90° 和 Z = 4。通过直接方法解析结构并在 3796 次观察到的反射上精炼为 R 1 值 0.0975。有一个[Fe III L 2 ]八面体阳离子单元，一个[Fe III Cl 4 ]四面体阴离子单元和0。5(C 2 H 5 OH) 2 作为溶剂分子在(1)的晶格的不对称单元中。有两种分子内 C–H ⋯ O 相互作用，晶体堆积通过离子间 C–H ⋯ Cl 和分子间 C–H ⋯ Cg 相互作用稳定。图形摘要 带有偶氮硫醚配体的铁 (III) 配合物的单晶 X 射线衍射研究，提出了 2-羟基-1-(2'-甲基硫代苯基偶氮)萘 (HL)，该配合物的晶体堆积，[Fe已发现 III L 2 ] + [Fe III Cl 4 ] - ( 1 ) 被离子间 C–H ⋯ Cl 和分子间 C–H ⋯ Cg 相互作用稳定。