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Title: Characterization of Reactive Organometallic Species via MicroED

Abstract

Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition-metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultrasensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as “Schwartz’s reagent”, a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic and diamagnetic transition-metal complexes.

Authors:
; ; ;  [1]; ; ;  [1]; ; ;  [1]; ORCiD logo; ORCiD logo [1]; ; ORCiD logo
  1. Department of Chemistry, University of California, Riverside, California 92521, United States
Publication Date:
Research Org.:
Univ. of California, Los Angeles, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1560723
Alternate Identifier(s):
OSTI ID: 1609011
Grant/Contract Number:  
FC02-02ER63421
Resource Type:
Published Article
Journal Name:
ACS Central Science
Additional Journal Information:
Journal Name: ACS Central Science Journal Volume: 5 Journal Issue: 9; Journal ID: ISSN 2374-7943
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Chemistry; Anions; Electron diffraction; Crystal structure; Physical and chemical processes; Molecular structure

Citation Formats

Jones, Christopher G., Asay, Matthew, Kim, Lee Joon, Kleinsasser, Jack F., Saha, Ambarneil, Fulton, Tyler J., Berkley, Kevin R., Cascio, Duilio, Malyutin, Andrey G., Conley, Matthew P., Stoltz, Brian M., Lavallo, Vincent, Rodríguez, José A., and Nelson, Hosea M. Characterization of Reactive Organometallic Species via MicroED. United States: N. p., 2019. Web. doi:10.1021/acscentsci.9b00403.
Jones, Christopher G., Asay, Matthew, Kim, Lee Joon, Kleinsasser, Jack F., Saha, Ambarneil, Fulton, Tyler J., Berkley, Kevin R., Cascio, Duilio, Malyutin, Andrey G., Conley, Matthew P., Stoltz, Brian M., Lavallo, Vincent, Rodríguez, José A., & Nelson, Hosea M. Characterization of Reactive Organometallic Species via MicroED. United States. doi:10.1021/acscentsci.9b00403.
Jones, Christopher G., Asay, Matthew, Kim, Lee Joon, Kleinsasser, Jack F., Saha, Ambarneil, Fulton, Tyler J., Berkley, Kevin R., Cascio, Duilio, Malyutin, Andrey G., Conley, Matthew P., Stoltz, Brian M., Lavallo, Vincent, Rodríguez, José A., and Nelson, Hosea M. Fri . "Characterization of Reactive Organometallic Species via MicroED". United States. doi:10.1021/acscentsci.9b00403.
@article{osti_1560723,
title = {Characterization of Reactive Organometallic Species via MicroED},
author = {Jones, Christopher G. and Asay, Matthew and Kim, Lee Joon and Kleinsasser, Jack F. and Saha, Ambarneil and Fulton, Tyler J. and Berkley, Kevin R. and Cascio, Duilio and Malyutin, Andrey G. and Conley, Matthew P. and Stoltz, Brian M. and Lavallo, Vincent and Rodríguez, José A. and Nelson, Hosea M.},
abstractNote = {Here we apply microcrystal electron diffraction (MicroED) to the structural determination of transition-metal complexes. We find that the simultaneous use of 300 keV electrons, very low electron doses, and an ultrasensitive camera allows for the collection of data without cryogenic cooling of the stage. This technique reveals the first crystal structures of the classic zirconocene hydride, colloquially known as “Schwartz’s reagent”, a novel Pd(II) complex not amenable to solution-state NMR or X-ray crystallography, and five other paramagnetic and diamagnetic transition-metal complexes.},
doi = {10.1021/acscentsci.9b00403},
journal = {ACS Central Science},
number = 9,
volume = 5,
place = {United States},
year = {2019},
month = {9}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record
DOI: 10.1021/acscentsci.9b00403

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Cited by: 3 works
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Works referencing / citing this record:

Single crystal growth of water-soluble metal complexes with the help of the nano-crystallization method
journal, January 2020

  • Alvarez, Ricardo; Nievergelt, Philipp P.; Slyshkina, Ekaterina
  • Dalton Transactions, Vol. 49, Issue 28
  • DOI: 10.1039/d0dt01236j