Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2′-bipyridine-κ2N,N′)(oxalato-κ2O1,O2)nickel(II)

Farka?ová; Nela.; ernák; Juraj.; Tomás; Milagros.; Falvello; Larry R.

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Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2′-bipyridine-κ2N,N′)(oxalato-κ2O1,O2)nickel(II)

机译：双（2,2'-联吡啶-κ2N，N'）（草酸-κ2O1，O2）镍（II）的新五水合物的合成，表征和晶体结构

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The reaction of NiCl2, K2C2O4·H2O and 2,2′-bipyridine (bpy) in water–ethanol solution at 281?K yields light-purple needles of the new pentahydrate of bis(2,2′-bipyridine)oxalatonickel(II), [Ni(C2O4)(C10H8N2)2]·5H2O or [Ni(ox)(bpy)2]·5H2O, while at room temperature, deep-pink prisms of the previously reported tetrahydrate [Ni(ox)(bpy)2]·4H2O [Román, Luque, Guzmán-Miralles & Beitia (1995), Polyhedron, 14, 2863–2869] were gathered. The asymmetric unit in the crystal structure of the new pentahydrate incorporates the discrete molecular complex [Ni(ox)(bpy)2] and five solvent water molecules. Within the complex molecule, all three ligands are bonded as chelates. The complex molecules are involved in an extended system of hydrogen bonds with the solvent water molecules. Additionally, π–π interactions also contribute to the stabilization of the extended structure. The dehydration of the pentahydrate starts at 323?K and proceeds in at least two steps as determined by thermal analysis.

机译：NiCl2，K2C2O4·H2O和2,2'-联吡啶（bpy）在水-乙醇溶液中于281？K的反应产生浅紫色的双（2,2'-联吡啶）草酰酮镍（II）五水合物，[Ni（C2O4）（C10H8N2）2]·5H2O或[Ni（ox）（bpy）2]·5H2O，而在室温下，先前报道的四水合物[Ni（ox）（bpy）2 ]·4H2O [Román，Luque，Guzmán-Miralles＆Beitia（1995），Polyhedron，14，2863-2869]被收集。新的五水合物的晶体结构中的不对称单元包含离散的分子复合物[Ni（ox）（bpy）2]和五个溶剂水分子。在复杂分子中，所有三个配体都作为螯合物键合。复杂分子参与了与溶剂水分子的氢键扩展系统。另外，π-π相互作用也有助于扩展结构的稳定。五水合物的脱水始于323？K，并通过热分析确定至少分两个步骤进行。

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《Acta crystallographica. Section C, Structural chemistry.》 |2014年第5期|共5页
作者
Farka?ová; Nela.; ernák; Juraj.; Tomás; Milagros.; Falvello; Larry R.;
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正文语种 eng
中图分类晶体学;
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crystal structure; TGA/DTA analysis; bis(2; 2′-bipyridine)(oxalato)nickel(II); pentahydrate; IR spectra; hydrogen bonding; π–π interactions;

机译：晶体结构;TGA / DTA分析;双（2;2′-联吡啶）（草酸）镍（II）;五水合物;红外光谱;氢键;π-π相互作用;

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1. Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2′-bipyridine-κ2N,N′)(oxalato-κ2O1,O2)nickel(II) [J] . Farka?ová, Nela., ernák, Acta crystallographica. Section C, Structural chemistry. . 2014,第5期

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2. Synthesis, crystal structure and magnetic properties of (acetato-κ2O,O′)bis(5,5′-dimethyl-2,2′-bipyridine-κ2N,N′)nickel(II) perchlorate monohydrate [J] . Nela Farka?ová, Juraj ?ernák, Larry R. Falvello, Acta crystallographica. Section C, Structural chemistry. . 2015,第4期

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Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2′-bipyridine-κ2N,N′)(oxalato-κ2O1,O2)nickel(II)

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