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A green approach to the preparation of triangular silver(I) 3,5-bis(trifluoromethyl)pyrazolate: crystal structures of two adducts with triethylammonium nitrate or benzoic acid
Transition Metal Chemistry ( IF 1.7 ) Pub Date : 2019-09-16 , DOI: 10.1007/s11243-019-00345-z
Rongrong Liu , Pingning Jin , Jing-Huo Chen , Guang Yang , Wenhua Zhang

An improved procedure is described herein for the synthesis of triangular Ag(I) 3,5-bis(trifluoromethyl)pyrazolate ({[3,5-(CF3)2Pz]Ag}3), which involves initial preparation of its adducts with triethylammonium nitrate or benzoic acid, namely {[3,5-(CF3)2Pz]Ag}3·(Et3NH·NO3)2 (1) and {[3,5-(CF3)2Pz]Ag}3·(PhCOOH)2 (2), followed by removal of the nitrate and benzoic acid by washing or extraction with water to afford the pristine trisilver complex {[3,5-(CF3)2Pz]Ag}3. X-ray diffraction analysis on 1 and 2 reveals that {[3,5-(CF3)2Pz]Ag}3, acting as a π-acidic host, can combine with guest molecules/ions (NO3−, PhCOOH) by weak Ag–O/C coordination bonds, π–π stacking and C–H···F interactions. Our proposed synthetic procedure for {[3,5-(CF3)2Pz]Ag}3 can be easily carried out at room temperature, without using complex Schlenk techniques or hazardous organic solvents such as benzene and toluene, thus representing a green and facile approach to this well-recognized π-acidic complex.

中文翻译:

一种制备三角银(I)3,5-双(三氟甲基)吡唑酸盐的绿色方法:两种与硝酸三乙基铵或苯甲酸加合物的晶体结构

本文描述了一种用于合成三角形 Ag(I) 3,5-双(三氟甲基)吡唑酸盐 ({[3,5-(CF3)2Pz]Ag}3) 的改进程序,该程序涉及用三乙铵对其加合物进行初始制备硝酸盐或苯甲酸,即{[3,5-(CF3)2Pz]Ag}3·(Et3NH·NO3)2(1)和{[3,5-(CF3)2Pz]Ag}3·(PhCOOH)2 (2),然后用水洗涤或萃取除去硝酸盐和苯甲酸,得到原始三银配合物{[3,5-(CF3)2Pz]Ag}3。1 和 2 的 X 射线衍射分析表明 {[3,5-(CF3)2Pz]Ag}3 作为 π 酸性主体,可以通过弱 Ag 与客体分子/离子(NO3-,PhCOOH)结合–O/C 配位键、π–π 堆积和 C–H…F 相互作用。我们提出的 {[3,5-(CF3)2Pz]Ag}3 合成程序可以很容易地在室温下进行,
更新日期:2019-09-16
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