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Characterization of Reactive Organometallic Species via MicroED

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 Rodriguez, Jose A. and Nelson, Hosea M. (2019) Characterization of Reactive Organometallic Species via MicroED. ACS Central Science, 5 (9). pp. 1507-1513. ISSN 2374-7943. PMCID PMC6764211. https://resolver.caltech.edu/CaltechAUTHORS:20190906-134149357

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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.


Item Type:Article
Related URLs:
URLURL TypeDescription
https://doi.org/10.1021/acscentsci.9b00403DOIArticle
https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6764211PubMed CentralArticle
ORCID:
AuthorORCID
Fulton, Tyler J.0000-0002-9343-2456
Stoltz, Brian M.0000-0001-9837-1528
Lavallo, Vincent0000-0001-8945-3038
Nelson, Hosea M.0000-0002-4666-2793
Additional Information:© 2019 American Chemical Society. This is an open access article published under an ACS AuthorChoice License, which permits copying and redistribution of the article or any adaptations for non-commercial purposes. Received: April 19, 2019; Published: September 6, 2019. The authors thank Michael R. Sawaya, Michael K. Takase, Michael J. Collazo, Marcus Gallagher-Jones, and Chih-Te Zee (University of California, Los Angeles) for technical expertise and inspirational discussions. This material is based upon work supported by the National Science Foundation Graduate Research Fellowship (to C.G.J. and A.S.) under Grant No. DGE-1650604. This work is funded by STROBE, an NSF STC under Grant No. DMR 1548924. This work was supported by the University of California, Riverside. The solid-state NMR measurements at 14.1 T were recorded on an instrument supported by the National Science Foundation (CHE-1626673). V.L. acknowledges support from the National Science Foundation (CHE-1455348). J.A.R. acknowledges support from the Arnold and Mabel Beckman Foundation, the Pew Charitable Trusts, the Searle Scholars Program, the U.S. Department of Energy (Grant No. DE-FC02-02ER63421), and the National Institutes of Health—National Institute of General Medical Sciences (Grant Nos. P41 GM102403 and R35 GM128867). H.M.N. acknowledges support from the David and Lucile Packard Foundation, the Alfred P. Sloan Foundation, and the Pew Charitable Trusts. The authors thank the Beckman Institute Resource Center for Transmission Electron Microscopy at Caltech. Author Contributions: C.G.J. and M.A. contributed equally. C.G.J. performed experiments, developed the sample preparation techniques, processed and refined structural data, prepared figures, and assisted with manuscript preparation. M.A. prepared samples, refined structural data, and assisted with manuscript and figure preparation. L.J.K. performed experiments, processed structural data, prepared figures, and assisted with manuscript preparation. J.F.K. prepared isolated and characterized compounds. A.S. processed and refined data, wrote and executed MATLAB code, prepared figures, and assisted in manuscript preparation. T.J.F. performed experiments and assisted with manuscript preparation. K.R.B. prepared isolated and characterized compounds. D.C. assisted in processing and refining structural data and provided crystallographic expertise. A.G.M. assisted in data collection. M.P.C. performed solid-state NMR experiments. B.M.S. designed experiments and assisted with manuscript preparation. V.L. designed experiments and assisted with manuscript preparation. J.A.R. performed experiments, developed sample preparation techniques, maintained the microscope, analyzed data, and assisted with manuscript preparation. H.M.N. conceived of the project, designed experiments, performed experiments, developed the sample preparation techniques, and assisted with manuscript and figure preparation. The authors declare no competing financial interest.
Funders:
Funding AgencyGrant Number
NSF Graduate Research FellowshipDGE-1650604
NSFDMR-1548924
NSFCHE-1626673
NSFCHE-1455348
Arnold and Mabel Beckman FoundationUNSPECIFIED
Pew Charitable TrustsUNSPECIFIED
Searle Scholars ProgramUNSPECIFIED
Department of Energy (DOE)DE-FC02-02ER63421
NIHP41 GM102403
NIHR35 GM128867
David and Lucile Packard FoundationUNSPECIFIED
Alfred P. Sloan FoundationUNSPECIFIED
University of California, RiversideUNSPECIFIED
Issue or Number:9
PubMed Central ID:PMC6764211
Record Number:CaltechAUTHORS:20190906-134149357
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20190906-134149357
Official Citation:Characterization of Reactive Organometallic Species via MicroED. Christopher G. Jones, Matthew Asay, Lee Joon Kim, Jack F. Kleinsasser, Ambarneil Saha, Tyler J. Fulton, Kevin R. Berkley, Duilio Cascio, Andrey G. Malyutin, Matthew P. Conley, Brian M. Stoltz, Vincent Lavallo, José A. Rodríguez, and Hosea M. Nelson. ACS Central Science 2019 5 (9), 1507-1513. DOI: 10.1021/acscentsci.9b00403
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:98492
Collection:CaltechAUTHORS
Deposited By: George Porter
Deposited On:06 Sep 2019 21:28
Last Modified:03 Oct 2019 21:41

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