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NMR Confirmation for Formation of [B_(12)H_(12)]^(2-) Complexes during Hydrogen Desorption from Metal Borohydrides

Hwang, Son-Jong and Bowman, Robert C., Jr. and Reiter, Joseph W. and Rijssenbeek, Job and Soloveichik, Grigorii L. and Zhao, Ji-Cheng and Kabbour, Houria and Ahn, Channing C. (2008) NMR Confirmation for Formation of [B_(12)H_(12)]^(2-) Complexes during Hydrogen Desorption from Metal Borohydrides. Journal of Physical Chemistry C, 112 (9). pp. 3164-3169. ISSN 1932-7447. https://resolver.caltech.edu/CaltechAUTHORS:20170719-065012031

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Abstract

^(11)B NMR spectroscopy has been employed to identify the reaction intermediates and products formed in the amorphous phase during the thermal hydrogen desorption of metal tetrahydroborates (borohydrides) LiBH_4, Mg(BH_4)_2, LiSc(BH_4)_4, and the mixed Ca(AlH_4)_(2-)LiBH_4 system. The ^(11)B magic angle spinning (MAS) and cross polarization magic angle spinning (CPMAS) spectral features of the amorphous intermediate species closely coincide with those of a model compound, closo-borane K2B_(12)H_(12) that contains the [B_(12)H_(12)]^(2-) anion. The presence of [B_(12)H_(12)]^(2-) in the partially decomposed borohydrides was further confirmed by high-resolution solution ^(11)B and ^1H NMR spectra after dissolution of the intermediate desorption powders in water. The formation of the closo-borane structure is observed as a major intermediate species in all of the metal borohydride systems we have examined.


Item Type:Article
Related URLs:
URLURL TypeDescription
http://dx.doi.org/10.1021/jp710894tDOIArticle
http://pubs.acs.org/doi/abs/10.1021/jp710894tPublisherArticle
ORCID:
AuthorORCID
Hwang, Son-Jong0000-0002-3210-466X
Bowman, Robert C., Jr.0000-0002-2114-1713
Additional Information:© 2008 American Chemical Society. Received 14 November 2007. Published online 13 February 2008. Published in print 1 March 2008. The authors express special thanks to Dr. Satish S. Jalisatgi (U. Missouri-Columbia) for generously providing the K_2B_(12)H_(12) and K_2B_(10)H_(10) compounds. This research was partially performed at the Jet Propulsion Laboratory, which is operated by the California Institute of Technology under contract with the NASA. This work was partially supported by DOE through Award Nos. DE-AI-01-05EE11105 and DE-FC3605GO15062. The NMR facility at Caltech was supported by the National Science Foundation (NSF) under Grant No. 9724240 and partially supported by the MRSEC Program of the NSF under Award No. DMR-0520565.
Funders:
Funding AgencyGrant Number
NASA/JPL/CaltechUNSPECIFIED
Department of Energy (DOE)DE-AI-01-05EE11105
Department of Energy (DOE)DE-FC3605GO15062
NSFDMR-9724240
NSFDMR-0520565
Issue or Number:9
Record Number:CaltechAUTHORS:20170719-065012031
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20170719-065012031
Official Citation:NMR Confirmation for Formation of [B12H12]2- Complexes during Hydrogen Desorption from Metal Borohydrides Son-Jong Hwang, Robert C. Bowman, Jr, Joseph W. Reiter, Job Rijssenbeek, Grigorii L. Soloveichik, Ji-Cheng Zhao, Houria Kabbour, and Channing C. Ahn The Journal of Physical Chemistry C 2008 112 (9), 3164-3169 DOI: 10.1021/jp710894t
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:79183
Collection:CaltechAUTHORS
Deposited By: Ruth Sustaita
Deposited On:19 Jul 2017 15:15
Last Modified:03 Oct 2019 18:17

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