Synthesis of Nickel(II) complex with 2,6-dichlorophenyl-substituted pyridylpyrazole

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The mononuclear nickel(II) complex [L2Ni(CH3OH)]Cl (I) was synthesized by the interaction of new ligand 2-(2,6-dichlorophenyl)-5-(pyridin-2-yl)-2,4-dihydro-3H-pyrazol-3-one (L) with nickel(II) chloride. The solvate of complex I with methanol [L2Ni(CH3OH)]Cl·3CH3OH and the initial ligand L were characterized by X-ray diffraction analysis (CCDC № 2314989 (I), 2314988 (L)). It was observed that ligand L exists in the pyrazolone form based on 1H NMR data, whereas in complex I, it is found in the pyrazolol form according to X-ray diffraction data. Complex I is a unique example of a pyrazolol complex in which the oxygen atom does not engage in coordinating with the transition metal ion to create the coordination polymer.

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作者简介

I. Nikovskii

Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences

编辑信件的主要联系方式.
Email: igornikovskiy@mail.ru
俄罗斯联邦, Moscow

E. Safiullina

Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences

Email: igornikovskiy@mail.ru
俄罗斯联邦, Moscow

Yu. Nelyubina

Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences; Moscow Institute of Physics and Technology

Email: igornikovskiy@mail.ru
俄罗斯联邦, Moscow; Dolgoprudny, Moscow Region

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2. Rice. 1. 1H NMR spectrum of ligand L in CDCl3.

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3. Fig. 2. General view of the ligand L (a) and the hydrogen-bonded cycle (b) in the crystal of L CH3OH with atoms represented by thermal vibration ellipsoids (p = 50%). The dotted lines show the intermolecular hydrogen bond.

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4. Fig. 3. General view of the [L2Ni(CH3OH)]+ complex cation in the [L2Ni(CH3OH)]Cl 3СH3OH crystal with atoms represented by thermal vibration ellipsoids (p = 50%). Hydrogen atoms, except for those belonging to the OH groups of the ligand L and the coordinated methanol molecule, are not shown, as are the chloride anion in the outer coordination sphere and the solvate methanol molecules; numbering is given only for the metal ion and heteroatoms.

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5. Scheme 1

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6. Scheme 2

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7. Scheme 3

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8. Scheme 4

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9. Scheme 5

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