Crystal structure of benzyltriethylammonium catena-(tetrakis-μ2- sulfido)silver(I)-tungsten(VI), [C13H22N][AgWS4]

Guo-Dong Tang, Jian-Ying Zhao, Zheng-Jing Jiang
2010 Zeitschrift für Kristallographie - New Crystal Structures  
C 13 H 22 AgNS 4 W, tetragonal, P4 3 2 1 2(no. 96), a =11.1942(7) Å, c =29.877(4) Å, V =3743.9 Å 3 , Source of material AgI (0.235 g, 1mmol) was added to dmf (6 ml) solution, the mixture was stirred at room temperature for 10 min, after which, a pale yellow solution was formed. Benzyltriethylammonium hydroxide (1 mmol, 0.209 g) was then added to the solution with stirring, the orange solution was formed. The solution was further stirred for about 20 min, and al ight yellow precipitate was
more » ... ecipitate was formed. The reaction mixture was filtered and the filtrate was then transfered to atest tube and carefully layed by 10 ml i-PrOH. Light yellow block-shaped crystals were obtained after 15 days. Experimental details Hydrogen atoms were positioned geometrically and refined using ariding model, with d(C-H) =0.93 -0.97 Å and with U iso(H) = 1.2 U eq(C) [1.5 Ueq(C) for the methyl group]. The value of the Flack parameter is -0.010(8), which confirms the determined absolute structure.
doi:10.1524/ncrs.2010.0174 fatcat:zuk6eionv5bc5fsu2unup2cxai