Novel tri/tetra-coordination dual-core copper [I] coordination compound blue-green materials and preparation method thereof
A four-coordination and complex technology, which is applied in the direction of luminescent materials, copper organic compounds, chemical instruments and methods, etc., can solve the problems of few literature reports
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Embodiment 1
[0037] Under argon atmosphere, equimolar [Cu[MeCN] 4 ][ClO 4 ] (186mg, 0.57mmol) and bis[diphenylphosphine]methane (219mg, 0.57mmol) were stirred and reacted at room temperature in 20mL dichloromethane solvent for 0.5 hours, and then added 5-tert-butyl -3-[6-methyl-2-pyridyl]-1,2,4-triazole ligand (124mg, 0.57mmol), continue to stir the reaction at room temperature for 4 hours, and then dissolve the solvent on a rotary evaporator Evaporate to dryness, and recrystallize with dichloromethane (4mL)-methanol (2mL)-ether (30mL) mixed solvent [volume ratio 2:1:15]. The crystalline product obtained by recrystallization was filtered, washed 3-4 times with 20 mL of ether, and dried under vacuum to obtain a off-white solid product—perchlorate[5-tert-butyl-3-[6-methyl-2 -pyridyl]-1,2,4-triazole]·bis[bis[diphenylphosphine]methane]copper[I] complex (236 mg, 0.18 mmol), yield 63%.
[0038] Elemental analysis calculated value (C 62 h 60 Cl 2 Cu 2 N 4 o 8 P 4 ) is (%): C56.80, H4.61...
Embodiment 2
[0044] Under argon atmosphere, copper perchlorate hexahydrate [Cu[ClO 4 ] 2 ·6H 2 O] (167mg, 0.45mmol) and excess copper powder (230mg, 3.62mmol) were stirred and reacted in 8mL of acetonitrile solvent for 20 minutes, and then added a solution of bis[diphenylphosphine]methane (347mg, 0.90mmol) in 12mL of dichloromethane , continue to stir and react for 1 hour, then add 5-tert-butyl-3-[6-methyl-2-pyridyl]-1,2,4-triazole ligand (195mg, 0.90mmol), continue at room temperature Stir the reaction for 3 hours, filter and evaporate the solvent to dryness on a rotary evaporator, and use dichloromethane (4mL)-methanol (2mL)-ether (30mL) mixed solvent [volume ratio 2:1:15] for recrystallization. The crystalline product obtained by recrystallization was filtered, washed 3-4 times with 25 mL of ether, and dried in vacuo to obtain a off-white solid product——perchlorate[5-tert-butyl-3-[6-methyl-2- Pyridyl]-1,2,4-triazole]·bis[bis[diphenylphosphine]methane]copper[I] complex (342mg, 0.26mmo...
Embodiment 3
[0048] Under argon atmosphere, equimolar [Cu[MeCN] 4 ][ClO 4 ] (164mg, 0.50mmol) and bis[diphenylphosphine]methane (193mg, 0.50mmol) were stirred and reacted at room temperature in 17mL dichloromethane solvent for 0.5 hours, and then added 5-trifluoromethane in the colorless and transparent reaction solution Base-3-[2-pyridyl]-1,2,4-triazole ligand (108mg, 0.50mmol), continue to stir and react at room temperature for 4.5 hours, then evaporate the solvent to dryness on a rotary evaporator, and use Dichloromethane (4mL)-methanol (2mL)-ether (30mL) mixed solvent [volume ratio 2:1:15] was used for recrystallization. The crystalline product obtained by recrystallization was filtered, washed 3-4 times with 18 mL of ether, and dried under vacuum to obtain a off-white solid product——perchlorate[5-trifluoromethyl-3-[2-pyridyl] -1,2,4-triazole] bis[bis[diphenylphosphine]methane]copper[I] complex (206mg, 0.17mmol),
[0049] The yield was 68%.
[0050] Elemental analysis calculated va...
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