We cover our recent work on low and high oxidation state as well as cluster Ir complexes where a wide variety of standard crystallization methods failed. For Ir(I), butane-1,4-diol can promote crystallization by hydrogen bonding to unpartnered basic hydrogen bonding groups on the complex. Two gel methods proved useful in the cluster cases. For the [Ir4(IMe)8H9]3+ cluster cation, we find the Keggin cluster anion [PW12O40]3− is most suitable. The related [Ir4(IMe)8(H)10][B(Arf)4]2 even gave large enough crystals (0.9 × 0.4 × 0.1 mm) for neutron diffraction, needed to locate the hydrides. For Ir(IV) and (V), CCl4 proves a useful precipitant that also tends to incorporate in the lattice. Finally, Ir(V) complexes were crystallized directly from the electrosynthetic solutions.
ASJC Scopus subject areas
- Physical and Theoretical Chemistry
- Inorganic Chemistry
- Materials Chemistry