研究目的
To synthesize and characterize new one-dimensional mercury(II) coordination polymers using a dispiro-dipyridyloxy-cyclotriphosphazene ligand, and to investigate their structural, thermal, and UV-vis absorption properties.
研究成果
The study successfully synthesized and characterized two new 1D mercury(II) coordination polymers with the ligand L, confirming κ2N binding mode and distorted tetrahedral geometry for Hg ions. UV-Vis experiments supported the 1:1 complex formation in solution, consistent with crystal structures. TGA showed good thermal stability, with L being more stable than the complexes. This work reinforces the utility of cyclotriphosphazene ligands in forming 1D polymers and provides insights into their optical and thermal properties.
研究不足
The study is limited to specific mercury salts (HgI2 and HgCl2) and the ligand L; other metal ions or ligands were not explored. The thermal stability is only up to 300°C, and the UV-Vis properties are investigated in solution state only, not in solid state. The crystal structures show distorted geometries, which might affect properties, and the supramolecular interactions are weak.
1：Experimental Design and Method Selection:
The study involved synthesizing coordination polymers by reacting the ligand L with HgI2 and HgCl2 in acetonitrile, followed by crystallization. Structural characterization was done using single crystal X-ray crystallography, elemental analysis, UV-Vis spectroscopy, and thermogravimetric analysis (TGA).
2：Sample Selection and Data Sources:
The ligand L was synthesized as per literature. Mercury salts (HgI2 and HgCl2) and solvents were purchased from commercial sources. Crystals of the complexes were grown from filtered solutions.
3：List of Experimental Equipment and Materials:
Equipment includes a Mettler Toledo TGA/SDTA 851 for TGA, Shimadzu 2101 UV-Vis spectrometer for electronic spectra, Bruker APEX II QUAZAR diffractometer for X-ray crystallography. Materials include hexachlorocyclotriphosphazene, ethane diol, 3-hydroxypyridine, HgI2, HgCl2, various solvents (THF, dichloromethane, n-hexane, acetonitrile, acetone, methanol), silica gel for chromatography.
4：Experimental Procedures and Operational Workflow:
Synthesis involved stirring L with Hg salts in acetonitrile at 80°C for 1 hour, filtering, and slow cooling to grow crystals. Crystals were washed and dried. For TGA, samples were heated from room temperature to 700°C at 10°C/min under N2. UV-Vis measurements were done in acetonitrile solutions using cuvettes and micropipettes. X-ray data collection involved mounting crystals on a diffractometer with Mo Kα radiation, followed by data integration and structure refinement.
5：UV-Vis measurements were done in acetonitrile solutions using cuvettes and micropipettes. X-ray data collection involved mounting crystals on a diffractometer with Mo Kα radiation, followed by data integration and structure refinement.
Data Analysis Methods:
5. Data Analysis Methods: X-ray data were processed using APEX2, SAINT, SADABS, SHELXT, and SHELXL software. UV-Vis data were analyzed for absorption bands and Job's plot to determine stoichiometry. TGA data were used to assess thermal stability.
独家科研数据包，助您复现前沿成果，加速创新突破
获取完整内容
