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Synthetic method and crystal structure of macrocyclic oxamide binuclear complex Cu-Ni

A technology of macrocyclic oxamide and dinuclear complexes, applied in the direction of organic chemistry, etc.

Inactive Publication Date: 2013-12-11
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, there are few reports on the synthesis of multinuclear complexes using macrocyclic oxamides as complex ligands.

Method used

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  • Synthetic method and crystal structure of macrocyclic oxamide binuclear complex Cu-Ni
  • Synthetic method and crystal structure of macrocyclic oxamide binuclear complex Cu-Ni
  • Synthetic method and crystal structure of macrocyclic oxamide binuclear complex Cu-Ni

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Embodiment 1

[0012] The synthesis of embodiment 1 complex:

[0013] Add dropwise 0.1mol / L Ni(ClO 4 ) 2 ·6H 2 O methanol solution 1mL, then add 1,10-phenanthroline (phen0.1mmol), react under reflux for 2 hours, cool and filter, the filtrate slowly evaporates at room temperature, after about 3 weeks, crystals are obtained in a beaker .

Embodiment 2

[0014] The structural determination of embodiment 2 complexes:

[0015] Select crystals of appropriate size, use Bruker Smart / Rigaku007 type X-ray single crystal diffractometer, at room temperature, use MoKα ray monochromatized by graphite monochromator ( ) as the incident light source, with The diffraction data were collected by scanning mode. The non-hydrogen atoms were solved by the direct method, and their coordinates and their anisotropic thermal parameters were corrected by the full-matrix least-squares method. The positions of the hydrogen atoms were obtained from theoretical hydrogenation and added to the structure refinement using ride-on reshaping positional parameters and fixed isotropic thermal parameters. All calculations were performed using the SHELXS-97 and SHELXL-97 program packages. The experimental conditions, structure analysis, correction method and crystallographic data of diffraction analysis are shown in Table 1. structure see figure 1 and figu...

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Abstract

The invention relates to a macrocyclic oxamide Cu-Ni binuclear complex and a preparation method thereof. The chemical formula of the macrocyclic oxamide Cu-Ni binuclear complex is [(CuL)Ni(CH3OH)(phen)(ClO4)2], wherein L=5,6,14,15-dibenzo-1,4,8,12-tetra-azacyclo-pentadecane-7,13-divinyl-2,3-diketone, and phen=1,10-phenanthroline. The macrocyclic oxamide Cu-Ni binuclear complex is in a one-dimensional chain structure. The preparation method comprises the following steps of: mixing CuL and Ni(ClO4)2.6H2O methanol solutions and phen, namely the 1,10-phenanthroline; and then reacting to obtain a target product.

Description

technical field [0001] The invention belongs to the field of science and technology of complexes, in particular to a synthesis method of macrocyclic oxamide heteronuclear complexes. technical background [0002] Since its inception, coordination chemistry has become a relatively mature subject after decades of development. And it occupies an important position in inorganic chemistry and even chemistry. In the 1970s, coordination chemistry and other disciplines of chemistry (such as organic chemistry, polymer chemistry, etc.) . With the rapid development of synthesis technology and testing technology, functional complexes with novel optical properties, electrical properties, magnetic properties and thermal properties have been synthesized and studied in depth. The research focus of today's coordination chemistry has gradually developed from complexes containing only a single central atom to polynuclear complexes containing multiple central atoms. In polynuclear complexes,...

Claims

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Application Information

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IPC IPC(8): C07F19/00
Inventor 周旭光孙亚秋
Owner TIANJIN POLYTECHNIC UNIV
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