Some crystal growth strategies for diffraction structure studies of iridium complexes

Liam S. Sharninghausen, Shashi Bhushan Sinha, Dimitar Y. Shopov, Gary W Brudvig, Robert H. Crabtree

Research output: Contribution to journalReview article

Abstract

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.

Original languageEnglish
Pages (from-to)183-188
Number of pages6
JournalInorganica Chimica Acta
Volume480
DOIs
Publication statusPublished - Aug 1 2018

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Iridium
Crystallization
iridium
Crystal growth
crystal growth
Hydrogen bonds
Diffraction
Butane
Neutron diffraction
diffraction
Hydrides
Anions
Cations
Negative ions
Gels
Positive ions
crystallization
Oxidation
Crystals
hydrogen

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

Cite this

Some crystal growth strategies for diffraction structure studies of iridium complexes. / Sharninghausen, Liam S.; Sinha, Shashi Bhushan; Shopov, Dimitar Y.; Brudvig, Gary W; Crabtree, Robert H.

In: Inorganica Chimica Acta, Vol. 480, 01.08.2018, p. 183-188.

Research output: Contribution to journalReview article

Sharninghausen, Liam S. ; Sinha, Shashi Bhushan ; Shopov, Dimitar Y. ; Brudvig, Gary W ; Crabtree, Robert H. / Some crystal growth strategies for diffraction structure studies of iridium complexes. In: Inorganica Chimica Acta. 2018 ; Vol. 480. pp. 183-188.
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