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 language | English |
|---|---|
| Pages (from-to) | 183-188 |
| Number of pages | 6 |
| Journal | Inorganica Chimica Acta |
| Volume | 480 |
| DOIs | |
| Publication status | Published - Aug 1 2018 |
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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 journal › Review article
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TY - JOUR
T1 - Some crystal growth strategies for diffraction structure studies of iridium complexes
AU - Sharninghausen, Liam S.
AU - Sinha, Shashi Bhushan
AU - Shopov, Dimitar Y.
AU - Brudvig, Gary W
AU - Crabtree, Robert H.
PY - 2018/8/1
Y1 - 2018/8/1
N2 - 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.
AB - 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.
UR - http://www.scopus.com/inward/record.url?scp=85054357060&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=85054357060&partnerID=8YFLogxK
U2 - 10.1016/j.ica.2018.05.017
DO - 10.1016/j.ica.2018.05.017
M3 - Review article
VL - 480
SP - 183
EP - 188
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
SN - 0020-1693
ER -