| Abstract: | Preparation and Crystal Structure of (n-Bu4N)3Ir(NCS)(SCN)5] The evaporated ethanolic extrakt of the reaction product of K3IrCl6] and HNO3, refluxed with an aqueous KSCN solution yields a mixture of the linkage isomers Ir(NCS)n(SCN)6?-n]3?, n = 0? 2, and small amounts of linkage isomeric chloropentarhodanoiridates(III), from which Ir(NCS)(SCN)5]3? has been isolated by ion exchange chromatography on DEAE-cellulose. The X-Ray structure determination on a single crystal of (n-Bu4N)3Ir(NCS)(SCN)5] (monoclinic, space group P 21/a, a = 17.513(5), b = 32.607(5), c = 23.661(5) Å, β = 94.757(5)°, Z = 8) confirms the existance of a heteroleptic hexakis(thiocyanato(N)-thiocyanato(S))iridate(III) with an Ir? N distance of 2.03 Å and Ir? S bond lengths between 2.29 and 2.38 Å. The SCN groups with angles between 166 and 175° are nearly linear with Ir? S? C angles from 99.9 to 109.4°. The Ir? N? C angles of the two crystallographic independent anions are 166 and 174°. |
