Structure of CrIIF(NCMe)2BF4. Rietveld refinement of a component of a physical mixture of unknown composition

Jae-Hyuk Her; Peter W. Stephens; Qiuying Zhu; Kendric J. Nelson; Joel S. Miller

doi:10.1039/B801509K

Structure of Cr^IIF(NCMe)₂BF₄. Rietveld refinement of a component of a physical mixture of unknown composition†

Jae-Hyuk Her,‡^a Peter W. Stephens,*^a Qiuying Zhu,^b Kendric J. Nelson^b and Joel S. Miller*^b

* Corresponding authors

^a Department of Physics & Astronomy, Stony Brook University, Stony Brook, NY, USA
E-mail: Peter.Stephens@sunysb.edu

^b Department of Chemistry, University of Utah, Salt Lake City, UT, USA
E-mail: jsmiller@chem.utah.edu

Abstract

The reaction of Cr^II(NCMe)₄(BF₄)₂ and [NBuⁿ₄][TCNE] (TCNE = tetracyanoethylene) in CH₂Cl₂ forms a solid that is a mixture of an amorphous reduced-TCNE containing phase(s) and a crystalline component. Rietveld refinement of the high-resolution, synchrotron X-ray powder pattern enabled the determination of the structure of the crystalline phase to be of Cr^IIF(NCMe)₂BF₄ composition and illustrates that this methodology can be used to determine the structure of a crystalline substance of unknown composition in the presence of confounding information from coexisting amorphous material. Cr^IIF(NCMe)₂BF₄ exhibits a 1-D chain structure with both μ-F and μ-BF₄⁻ linkages that forms a nonplanar 6-membered FCrFBFCr ring. Cr^IIF(NCMe)₂BF₄ possesses a previously unknown structure type and is a potential source of Cr^IIF⁺ for synthesis applications.

This article is part of the themed collection: CrystEngComm celebrates it's 10th anniversary with the publication of a theme issue containing articles written by Board members - old and new

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Article information

DOI: https://doi.org/10.1039/B801509K
Article type: Communication
Submitted: 28 Jan 2008
Accepted: 17 Mar 2008
First published: 10 Apr 2008

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CrystEngComm, 2008,10, 1728-1730

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Structure of Cr^IIF(NCMe)₂BF₄. Rietveld refinement of a component of a physical mixture of unknown composition

J. Her, P. W. Stephens, Q. Zhu, K. J. Nelson and J. S. Miller, CrystEngComm, 2008, 10, 1728 DOI: 10.1039/B801509K

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