研究目的
To synthesize and characterize new cuprous complexes with benzoxazole ligands, and investigate their structural regulation and photoluminescence properties influenced by different ligands and halogen/pseudohalide ions.
研究成果
Four new cuprous complexes with benzoxazole ligands were synthesized and characterized, showing four-coordinated copper(I) ions with slightly distorted tetrahedral geometry. The structure was regulated by different ligands and halogen/pseudohalide ions, leading to varied coordination modes. Photoluminescence analysis revealed that complexes 1, 3, and 4 exhibit two emission peaks attributed to MLCT, XMCT, and 3CC emissions, while complex 2 shows only one peak. These complexes show potential as luminescent or photochemical materials.
研究不足
The study is limited to specific benzoxazole ligands and copper halides/pseudohalides; other ligands or metal ions were not explored. The photoluminescence properties were only measured in solid state, and potential applications in solution or other environments were not investigated. The purity of complexes was high but not absolute, and differences in intensity in PXRD may indicate preferred orientation effects.
1:Experimental Design and Method Selection:
The study involved synthesizing cuprous complexes using different benzoxazole ligands (2-PBO, 4-PBO, BBO) and copper halides/pseudohalides (CuI, CuBr, CuSCN) through methods like natural volatilization, solvothermal, and interfacial reactions under nitrogen atmosphere. Structural analysis was performed using X-ray crystallography, and photophysical properties were measured.
2:Sample Selection and Data Sources:
Ligands were synthesized based on reported methods, and complexes were prepared with specific molar ratios. Single crystals were grown for X-ray diffraction studies.
3:List of Experimental Equipment and Materials:
Equipment included Carlo Erba 1106 elemental analyzer, Nicolet FT-VERTEX 70 spectrometer, Mercury plus 400 MHz NMR spectrometer, Shimadzu UV-2600 spectrometer, Siemens D5005 diffractometer, Edinburgh FLS980 spectrometer, and Bruker APEXII area detector. Materials included CuI, CuBr, CuSCN, NH4SCN, solvents like MeOH, CH3CN, DMF, DMSO, and synthesized ligands.
4:Experimental Procedures and Operational Workflow:
For each complex, ligands and copper salts were mixed in specific solvents, heated or allowed to evaporate to form crystals. Crystals were characterized by elemental analysis, IR, NMR, UV-Vis, PXRD, and photoluminescence measurements. X-ray data collection and refinement were done using SMART, SAINT, and SHELXTL programs.
5:Data Analysis Methods:
Data were analyzed using software for crystallography (e.g., SHELXTL), and photophysical parameters like emission lifetimes and quantum yields were calculated using standard equations.
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UV-Vis spectrometer
UV-2600
Shimadzu
Recording UV-Vis absorption spectra
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X-ray diffractometer
D5005
Siemens
Recording powder X-ray diffraction patterns with Cu-Kα radiation
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spectrometer
FLS980
Edinburgh
Recording photoluminescence spectra, emission lifetimes, and absolute emission quantum yields equipped with an integrating sphere
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area detector
APEXII
Bruker
Collecting intensity data for crystal structure determination with MoKα radiation
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elemental analyzer
1106
Carlo Erba
Elemental analysis for carbon, hydrogen, and nitrogen content
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FT-IR spectrometer
VERTEX 70
Nicolet
Recording IR spectra from 4000 to 400 cm?1 using KBr pellets
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NMR spectrometer
Mercury plus 400 MHz
Obtaining 1H NMR spectra with TMS as internal standard and DMSO-d6 as solvent
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