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Self-assembly of heteroleptic dinuclear silver(i) complexes bridged by bis(diphenylphosphino)ethyne†
Dalton Transactions ( IF 3.5 ) Pub Date : 2017-12-20 00:00:00 , DOI: 10.1039/c7dt03923a
Sarah Keller 1, 2, 3, 4 , Timothy N. Camenzind 1, 2, 3, 4 , Johannes Abraham 1, 2, 4, 5 , Alessandro Prescimone 1, 2, 3, 4 , Daniel Häussinger 1, 2, 4, 5 , Edwin C. Constable 1, 2, 3, 4 , Catherine E. Housecroft 1, 2, 3, 4
Affiliation  

We present a study of the self-assembling behaviour in solution of Ag[PF6] with one equivalent of an N^N ligand (N^N = 6,6′-dimethyl-2,2′-bipyridine (6,6′-Me2bpy) or 2,2′:6′,2′′-terpyridine (tpy)), together with either 0.5 or one equivalent of the bridging ligand bis(diphenylphosphino)ethyne (dppa). Each product contains a dinuclear cation, with one or two dppa ligands bridging the two Ag+ centres; 6,6′-Me2bpy and tpy, respectively, act as chelating ligands. The compounds have been analysed in solution using NMR spectroscopic methods (1H, 1H{31P}, COSY, NOESY, 13C, HMQC and HMBC), including room and low temperature measurements. 31P{1H} NMR spectra recorded at different temperatures allow a deeper insight into the dynamic equilibrium processes. In addition, solution 31P–109Ag HSQC spectroscopic measurements were performed and show, inter alia, the ratio of the splitting in the F1 dimension and the 1J31P–109Ag coupling constant in the fully coupled HSQC. Single crystal X-ray diffraction yielded two pseudo-polymorphic structures for the doubly-bridged [Ag2(dppa)2(tpy)2][PF6]2 and one for the singly-bridged [Ag2(dppa)(6,6′-Me2bpy)2][PF6]2.

中文翻译:

由双(二苯基膦基)乙炔桥接 的杂配双核银(i)配合物的自组装

我们提出了在Ag [PF 6 ]与一当量的N ^ N配体(N ^ N = 6,6'-二甲基-2,2'-联吡啶(6,6' -Me 2 bpy)或2,2':6',2''-叔吡啶(tpy)),以及0.5或1当量的桥联配体双(二苯基膦基)乙炔(dppa)。每个产物都包含双核阳离子,带有一个或两个dppa配体桥接两个Ag +中心。6,6'-Me 2 bpy和tpy分别充当螯合配体。已使用NMR光谱法(1 H,1 H { 31 P},COSY,NOESY,13 C,HMQC和HMBC)在溶液中分析了化合物,包括室温和低温测量。在不同温度下记录的31 P { 1 H} NMR光谱可让您更深入地了解动态平衡过程。此外,还进行了溶液31 P– 109 Ag HSQC光谱测量,除其他外,显示了F1尺寸的分光比与完全耦合HSQC中1 J 31 P– 109 Ag耦合常数的比值。单晶X射线衍射,得到两个伪多晶型结构的双桥接将[Ag 2(DPPA) 2(TPY) 2 ] [PF 6 ] 2,一个用于单桥接将[Ag 2(dppa)(6,6'-Me 2 bpy)2 ] [PF 6 ] 2
更新日期:2017-12-20
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