Organic phosphine copper nanocluster crystals and preparation method thereof
An organophosphine and cluster technology, applied in the field of organophosphine copper nano-cluster crystals and its synthesis, can solve the problems of difficult to accurately characterize the molecular structure, complex synthesis methods, poor crystallinity, etc., and achieve short reaction time and low preparation cost Low, high yield effect
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[0018] Specific steps are as follows:
[0019] (1). [Cu 2 (dppy) 3 (MeCN)] (ClO 4 ) 2 preparation of
[0020] Add 20 mL of MeCN, copper powder (200 mg, 3.1 mmol), dppy (1460 mg, 5.5 mmol) and [Cu(MeCN) 4 ]ClO 4 (1170 mg, 3.6 mmol), stirred for 1.5 h and filtered with suction. The filtrate was transferred to a dry 100 mL round bottom flask and concentrated to approximately 5 mL by rotary evaporation in a water bath at 40 °C. Add diethyl ether to the above concentrated solution until white turbidity appears, let the crystals crystallize fully, then filter with suction, wash the solid with a small amount of diethyl ether, continue to drain it and dry it at room temperature to obtain a white solid product [Cu 2 (dppy) 3 (MeCN)] (ClO 4 ) 2 (1770 mg, 1.5 mmol), with an average yield of 85%.
[0021] (2). [Cu 7 (dppy) 6 ](ClO 4 ) 2 and [Cu 4 (dppy) 4 Cl 2 ](ClO 4 ) Preparation of nanocluster crystals
[0022] In a nitrogen atmosphere, 0.2 mmol [Cu 2 (dppy) 3 (...
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