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

doi:10.1016/j.ica.2018.05.017

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

Yale University

Research output: Contribution to journal › Review article › peer-review

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(Ar^f)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	https://doi.org/10.1016/j.ica.2018.05.017
Publication status	Published - Aug 1 2018

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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title = "Some crystal growth strategies for diffraction structure studies of iridium complexes",

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.",

author = "Sharninghausen, {Liam S.} and Sinha, {Shashi Bhushan} and Shopov, {Dimitar Y.} and Brudvig, {Gary W.} and Crabtree, {Robert H.}",

year = "2018",

month = aug,

day = "1",

doi = "10.1016/j.ica.2018.05.017",

language = "English",

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journal = "Inorganica Chimica Acta",

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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.

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JO - Inorganica Chimica Acta

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