Synthetic and Structural Studies on Copper 1H-[1,10]-Phenanthrolin-2-one Coordination Complexes: Isolation of a Novel Intermediate During 1,10- Phenanthroline Hydroxylation

Katherine B. Szpakolski; Kay Latham; Colin J. Rix; Jonathan M. White; Boujemaa Moubaraki; Keith S. Murray

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Synthetic and Structural Studies on Copper 1H-[1,10]-Phenanthrolin-2-one Coordination Complexes: Isolation of a Novel Intermediate During 1,10- Phenanthroline Hydroxylation

机译：1H- [1,10]-菲咯啉-2-酮铜配合物的合成与结构研究：1,10-菲咯啉羟基化过程中新型中间体的分离

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The synthesis and crystal structure elucidation of a novel dinuclear heteroleptic copper(II) complex has led to an alternative mechanism in the formation of covalent hydrates. During further studies on the synthesis and properties of [Cu2ACHTUNGTRENUNG(ophen)2] (1), a dinuclear complex of copper(I) with 1H-[1,10]-phenanthrolin-2-one (Hophen), two intermediates/alternative products 2 and 3 were isolated. The dinuclear, antiferromagnetic complex [Cu2ACHTUNGTRENUNG(ophen)2ACHTUNGTRENUNG(phen)2]·ACHTUNGTRENUNG(NO3)2·9H2O (3, phen=1,10-phenanthroline) contains two five-coordinate copper(II) ions, both with trigonal-bipyramidal coordination, which are bridged together through deprotonated hydroxyl groups with a Cu-Cu non-bonding distance of 3.100 . Complex [CuACHTUNGTRENUNG(phen)2ACHTUNGTRENUNG(H2O)]·- ACHTUNGTRENUNG(NO3)2 (2) is a polymorph of a previously reported material. The occurrence of 2 and 3 has led us to propose a variation to the Gillard mechanism for the formation of covalent hydrates in bidentate N-heterocycles in which the attacking nucleophile may be the deprotonated form of 2, [Cu- ACHTUNGTRENUNG(phen)2(OH)], rather than free OH.

机译：新型双核杂多铜（II）配合物的合成和晶体结构的阐明已导致形成共价水合物的另一种机制。在进一步研究[Cu2ACHTUNGTRENUNG（ophen）2]（1）的过程中，这是一种铜（I）与1H- [1,10]-菲咯啉-2-酮（Hophen）的双核配合物，两种中间体/替代物分离出产物2和3。双核反铁磁复合物[Cu2ACHTUNGTRENUNG（ophen）2ACHTUNGTRENUNG（phen）2]·ACHTUNGTRENUNG（NO3）2·9H2O（3，phen = 1,10-phenothroline）包含两个五个五配位的铜离子（II）双锥体配位，通过去质子化的羟基桥接在一起，Cu-Cu非键距为3.100。复合物[CuACHTUNGTRENUNG（phen）2ACHTUNGTRENUNG（H2O）]-ACHTUNGTRENUNG（NO3）2（2）是先前报道的材料的多晶型物。 2和3的出现使我们提出了吉拉德机制的变体，该机制用于在双齿N杂环中形成共价水合物，其中攻击性亲核试剂可能是2的去质子化形式[Cu- ACHTUNGTRENUNG（phen）2（ OH）]，而不是游离的OH。

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《Chemistry: A European journal》 |2010年第5期|共6页
作者
Katherine B. Szpakolski; Kay Latham; Colin J. Rix; Jonathan M. White; Boujemaa Moubaraki; Keith S. Murray;
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正文语种 eng
中图分类应用化学;
关键词
copper; hydroxylation; nitrogen heterocycles; reaction mechanisms; structure elucidation;

机译：铜;羟基化;氮杂环;反应机理;结构阐明;

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1. Synthetic and Structural Studies on Copper 1H-[1,10]-Phenanthrolin-2-one Coordination Complexes: Isolation of a Novel Intermediate During 1,10- Phenanthroline Hydroxylation [J] . Katherine B. Szpakolski, Kay Latham, Colin J. Rix, Chemistry: A European journal . 2010,第5期

机译：1H- [1,10]-菲咯啉-2-酮铜配合物的合成与结构研究：1,10-菲咯啉羟基化过程中新型中间体的分离
2. Synthetic study of the ternary copper(II)/maleamate(-1)/1,10-phenanthroline reaction system: Mononuclear, dinuclear and polymeric complexes [J] . Lazarou KN, Perlepes SP, Psycharis V, Polyhedron: The International Journal for Inorganic and Organometallic Chemistry . 2008,第9a10期

机译：铜（II）/马来酸（-1）/ 1,10-菲咯啉三元反应体系的合成研究：单核，双核和聚合物络合物
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8. Structural Dependence of the Luminescence from Bis(substituted-benzenethiol)-(2,9-dimethyl-1,10- phenanthroline)zinc(II) Complexes [R] . Jordan, K. J., Wacholtz, W. F., Crosby, G. A. 1989

机译：双（取代苯硫酚） - （2,9-二甲基-1,10-菲咯啉）锌（II）配合物发光的结构依赖性

Synthetic and Structural Studies on Copper 1H-[1,10]-Phenanthrolin-2-one Coordination Complexes: Isolation of a Novel Intermediate During 1,10- Phenanthroline Hydroxylation

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