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Tetranuclear copper cluster compound synthesized through in-situ ligand reaction, and synthetic method and application thereof

A technology of in-situ ligands and synthesis methods, which is applied to the magnetic properties of copper organic compounds, organic materials/organic magnetic materials, etc., can solve the problems of rare and rare cluster compounds, and achieves easy operation, high yield, simple method effect

Inactive Publication Date: 2015-09-09
GUANGZHOU VOCATIONAL COLLEGE OF TECH & BUSINESS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In situ ligand reaction can obtain some novel organic ligands that cannot be synthesized by traditional methods. Although there are many reports on in situ ligand reaction, most of them are accidental under the conditions of hydrothermal, solvothermal and high temperature. found that in situ ligand reactions under mild conditions are relatively rare, and rational synthesis of clusters using in situ ligand reactions under mild conditions is even rarer

Method used

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  • Tetranuclear copper cluster compound synthesized through in-situ ligand reaction, and synthetic method and application thereof
  • Tetranuclear copper cluster compound synthesized through in-situ ligand reaction, and synthetic method and application thereof
  • Tetranuclear copper cluster compound synthesized through in-situ ligand reaction, and synthetic method and application thereof

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Experimental program
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Embodiment 1

[0034] A kind of synthetic method of the tetranuclear copper cluster compound of in-situ ligand reaction, comprises the following steps:

[0035] (1) 0.5mmol Cu(ClO 4 )·6H 2 O crystals and 0.5 mmol 2-cyanopyrimidine were dissolved in 20 ml of methanol, and after stirring for 10 minutes, solution A was obtained;

[0036] (2) 1.0mmol pyrazole was dissolved in 10ml methanol to prepare solution B;

[0037] (3) Heat solution A to 60°C, then add solution B to solution A, keep at 60°C for 20 minutes, cool to room temperature after reaction, filter, let stand at room temperature for 5-8 days, there are a lot of dark blue blocks Like crystals are precipitated, the crystals are separated, washed and dried to obtain tetranuclear copper clusters. The cluster yield was 45% based on copper.

[0038] Elemental analysis theoretical value: C, 31.89; H, 2.85; N, 22.32; experimental value: C, 31.76; H, 2.98; N, 22.28.

[0039] In this embodiment, the molar ratio of copper perchlorate hexahy...

Embodiment 2

[0041] The quadrinuclear copper cluster obtained in embodiment 1 is characterized and tested for performance:

[0042] (1) Structural characterization: select a single crystal with a suitable size, and under the condition of 293K, the X-ray diffraction data is on the Brucker Apex CCD surface detector, using Mo Kα radiation Collected in an omega scan and corrected for LP factors. Use SAINT + The program restores the data, and the absorption correction uses the SADAB program. Use the direct method to solve the structure, then use the difference Fourier method to find the coordinates of all non-hydrogen atoms, and use the theoretical hydrogenation method to obtain the hydrogen atom positions The structure was corrected using the method of least squares. The calculation work is done on PC with SHELXTL program package. Detailed crystallographic and structural revision data are shown in Table 1.

[0043] Table 1 Crystallographic parameter list

[0044]

[0045]

[0046...

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Abstract

The invention discloses a tetranuclear copper cluster compound synthesized through in-situ ligand reaction, and a synthetic method and application thereof. The cluster compound has a general chemical formula of Cu4(pymtz)2(pz)4(MeOH)2(ClO4)2, wherein pymtz represents 1-pyrazolyl-pyrimidine-2-azomethine, pz represents a pyrazolyl group, and MeOH is methanol. The cluster compound is of an annular structure and is constructed from polydentate nitrogen-containing ligand formed by cheap and easily available 2-cyanopyrimidine and pyrazole through in-situ nucleophilic addition reaction; the synthetic method is simple, has high yield and uses cheap raw materials; and the tetranuclear copper cluster compound has potential application prospect in the field of molecule-based magnetic materials.

Description

technical field [0001] The invention relates to a copper cluster compound and a synthesis method thereof, in particular to a tetranuclear copper cluster compound reacted with in-situ ligands, a synthesis method and application thereof. Background technique [0002] In recent years, the synthesis and properties of multinuclear transition metal clusters have become one of the research hotspots in the field of coordination chemistry and organometallic chemistry, because such metal clusters have important functions in molecular and ion exchange, adsorption, selective catalysis, optics and Molecular-based magnetic materials and other fields have potential application value. For the synthesis of multinuclear clusters, the selection of organic bridging ligands is very important. Common organic bridging ligands include carboxylic acids, pyridyl alcohols containing multiple hydroxyl groups, and imidazole alcohols. Most of these organic ligands are purchased through commercial channe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/08H01F1/42
Inventor 郑凌玲胡升
Owner GUANGZHOU VOCATIONAL COLLEGE OF TECH & BUSINESS