Abstract
The reaction of CrII(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 CrIIF(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. CrIIF(NCMe)2BF4 exhibits a 1-D chain structure with both μ-F and μ-BF4− linkages that forms a nonplanar 6-membered FCrFBFCr ring. CrIIF(NCMe)2BF4 possesses a previously unknown structure type and is a potential source of CrIIF+ for synthesis applications.
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