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双[μ-双(二苯基膦基)甲烷-κ(2)P:P']双[(异喹啉-κN)银(I)]双(三氟甲磺酸酯)-异喹啉(1/1)

Bis[μ-bis-(diphenyl-phosphan-yl)methane-κ(2)P:P']bis-[(isoquinoline-κN)silver(I)] bis-(trifluoro-methane-sulfonate)-isoquinoline (1/1).

作者信息

Huang Xu, Li Jing, Qiu Qi-Ming, Liu Min, Jin Qiong-Hua

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2012 Aug 1;68(Pt 8):m1022-3. doi: 10.1107/S1600536812029236. Epub 2012 Jul 4.

Abstract

The title complex, Ag(2)(C(25)H(22)P(2))(2)(C(9)H(7)N)(2)(2)·C(9)H(7)N, was prepared by the reaction of silver(I) trifluoro-methane-sulfonate with isoquinoline and bis-(diphenyl-phosphan-yl)methane (dppm). The dinuclear mol-ecule is located about a center of inversion and the Ag(I) atom is coordinated by two dppm P atoms and one isoquinoline N atom, forming an eight-membered metalla ring. In addition, in the asymmetric unit, there is a half-mol-ecule of isoquinoline located about a center of inversion. Since this mol-ecule does not possess this symmetry, for one position in the ring there is superposition of both a C atom of a C-H group and the isoquinoline N atom. In the structure, the Ag-P distances [2.4296 (9) and 2.4368 (9) Å] agree with the corresponding distances in related structures, while the Ag-N bond length [2.489 (3) Å] is slightly longer than that in related structures. On the other hand, the P-Ag-P angle [156.44 (3)°] is much larger than the corresponding angles in related structures. The trifluoro-methane-sulfonate anions do not coordinate to Ag(I) atoms. As is usually found for these anions, the -CF(3) group is disordered over two orientations [occupancies = 0.57 (12) and 0.43 (12)].

摘要

标题配合物Ag₂(C₂₅H₂₂P₂)₂(C₉H₇N)₂₂·C₉H₇N是通过三氟甲磺酸银(I)与异喹啉和双(二苯基膦基)甲烷(dppm)反应制备的。双核分子位于一个对称中心上,Ag(I)原子由两个dppm的P原子和一个异喹啉的N原子配位,形成一个八元金属环。此外,在不对称单元中,有一个位于对称中心上的异喹啉半分子。由于该分子不具有这种对称性,环中的一个位置存在一个C-H基团的C原子和异喹啉的N原子的叠加。在结构中,Ag-P键长[2.4296 (9)和2.4368 (9) Å]与相关结构中的相应键长一致,而Ag-N键长[2.489 (3) Å]比相关结构中的略长。另一方面,P-Ag-P角[156.44 (3)°]比相关结构中的相应角度大得多。三氟甲磺酸根阴离子不与Ag(I)原子配位。正如通常在这些阴离子中发现的那样,-CF₃基团在两个取向上无序[占有率 = 0.57 (12)和0.43 (12)]。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/17a9/3414098/5703a0fde2dd/e-68-m1022-fig1.jpg

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