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.
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.Attached Files
Published - acscentsci.9b00403.pdf
Submitted - characterization-of-reactive-organometallic-species-via-micro-ed.pdf
Supplemental Material - oc9b00403_si_001.pdf
Supplemental Material - oc9b00403_si_002.mp4
Supplemental Material - oc9b00403_si_003.mp4
Supplemental Material - oc9b00403_si_004.cif
Supplemental Material - oc9b00403_si_005.cif
Supplemental Material - oc9b00403_si_006.cif
Supplemental Material - oc9b00403_si_007.cif
Supplemental Material - oc9b00403_si_008.cif
Supplemental Material - oc9b00403_si_009.cif
Supplemental Material - oc9b00403_si_010.cif
Supplemental Material - oc9b00403_si_011.cif
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Additional details
- PMCID
- PMC6764211
- Eprint ID
- 98492
- Resolver ID
- CaltechAUTHORS:20190906-134149357
- DGE-1650604
- NSF Graduate Research Fellowship
- DMR-1548924
- NSF
- CHE-1626673
- NSF
- CHE-1455348
- NSF
- Arnold and Mabel Beckman Foundation
- Pew Charitable Trusts
- Searle Scholars Program
- DE-FC02-02ER63421
- Department of Energy (DOE)
- P41 GM102403
- NIH
- R35 GM128867
- NIH
- David and Lucile Packard Foundation
- Alfred P. Sloan Foundation
- University of California, Riverside
- Created
-
2019-09-06Created from EPrint's datestamp field
- Updated
-
2022-02-23Created from EPrint's last_modified field