Preparation and Characterization of cis- and trans-[Ir(tn)2Cl2]CF3SO3 and of [Ir(tn)3]Cl3 (tn=propane-1,3-diamine)

Michael Brorson, Frode Galsbøl, Kim Simonsen, Lars K. Skov, Inger Søtofte

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Procedures are given for the preparation and isolation of cis- and trans-[Ir(tn)2Cl2]CF3SO3 and of [Ir(tn)3]Cl3, (tn=propane-1,3-diamine). The compounds were prepared by the use of Ir(thtp)3Cl3 (thtp=tetrahydrothiophene) as starting material, using either DMSO or neat tn as solvent. A procedure for the preparation of [Rh(tn)3]Cl3 in quantitative yield from Rh(thtp)3Cl3 is also given. The complexes were characterized by 1H and 13C NMR and by UV/VIS spectroscopy. The conformation of the six-membered chelate rings of [Ir(tn)3]3+ in the solid state was determined by single-crystal X-ray diffraction of [Ir(tn)3] [Co(CN)6] x 5H2O. The three chelate rings all adopt the energetically favoured chair conformation; however, the overall idealized symmetry is C1. A comparative ligand field analysis, based on Gaussian resolution of the solution UV/VIS spectra for a number of homoleptic [M(N6)]3+ (M=CoIII, RhIII, IrIII) complexes, is also presented.
Original languageEnglish
JournalActa Chemica Scandinavica
Pages (from-to)1017-1023
Publication statusPublished - 1998

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