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Correction: Synthesis of Ca(PF6)2, formed via nitrosonium oxidation of calcium
Evan N.
Keyzer
a,
Peter D.
Matthews
ab,
Zigeng
Liu
a,
Andrew D.
Bond
a,
Clare P.
Grey
*a and
Dominic S.
Wright
*a
aDepartment of Chemistry, University of Cambridge, Lensfield Road, Cambridge, CB2 1EW, UK. E-mail: cpg27@cam.ac.uk; dsw1000@cam.ac.uk
bSchool of Chemistry, University of Manchester, Oxford Road, Manchester, M13 9BL, UK
First published on 16th October 2018
Abstract
Correction for ‘Synthesis of Ca(PF6)2, formed via nitrosonium oxidation of calcium’ by Evan N. Keyzer et al., Chem. Commun., 2017, 53, 4573–4576.
In the original article, Fig. 2 shows the structure of a Ca(PF6)2 species. Upon further analysis, the authors discovered that the structure is in fact [(Ca⊂15-crown-5)4(SiF6)2(CH3CN)2]4+(PF6−)4, with bridging SiF62− ligands rather than bridging PF6−. It appears that this error arose simply from picking a minor decomposition product during X-ray analysis as SiF62− was not observed in the 19F NMR spectrum of the sample. The SiF62− anion presumably arises from scavenging from the glass reaction vessel. The elemental analysis of this compound reported in the paper is of the mixture of products. A corrected CIF has been deposited at the CCDC (CCDC 1529827). This error does not affect the conclusion of the paper. A modified Fig. 2 is provided below, showing another example of a pure Ca(PF6)2 species (2a) produced using the identical procedure: [Ca⊂(15-crown-5)(CH3CN)3]2+[Ca⊂(15-crown-5)2]2+(PF6−)4 (CCDC 1556067). Again, the 19F and 31P NMR spectra show no evidence of decomposition to PO2F2− or SiF62−. Bulk purity of this sample was confirmed by elemental analysis [anal. calcd for C36H69Ca2F24N3O15P4 (2a): C, 29.95; H, 4.82; N, 2.91; P, 8.58; found: C, 28.81; H, 4.83; N, 3.01; P, 8.86].
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| Fig. 1 Crystal structure of 2a. Protons and disorder have been omitted for clarity (Ca, dark blue; C, grey; F, yellow; N, light blue; O, red; P, orange). | ||
The authors apologise for these errors and any consequent inconvenience to editors and readers.
The Royal Society of Chemistry apologises for these errors and any consequent inconvenience to authors and readers.
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