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DOI: 10.1039/C9DT90173F (Correction) Dalton Trans., 2019, 48, 12755-12756

Correction: Substituents drive ligand rearrangements, giving dinuclear rather than mononuclear complexes, and tune CoII/III redox potential†

Fabrice N. H. Karabulut , Humphrey L. C. Feltham and Sally Brooker *
Department of Chemistry and MacDiarmid Institute of Advanced Materials and Nanotechnology, University of Otago, PO Box 56, Dunedin 9054, New Zealand. E-mail: sbrooker@chemistry.otago.ac.nz

Received 29th July 2019 , Accepted 29th July 2019

First published on 9th August 2019

Abstract

Correction for ‘Substituents drive ligand rearrangements, giving dinuclear rather than mononuclear complexes, and tune CoII/III redox potential’ by Fabrice N. H. Karabulut et al., Dalton Trans., 2018, 47, 11749–11759, DOI: 10.1039/c8dt01502c.

Unfortunately many corrections need to be made to both the manuscript and ESI file. For optimal clarity, the key points are summarised in the bullet points below, with more details provided below that (and for the corrected ESI tables and figures please see the corrected ESI file, republished 29th July 2019).

1. There were numerous errors in the reporting of the elemental analysis and TGA data for this paper (resulting in a revised solvent content for the bulk samples), and missed recrystallisation steps in the experimental section (after which yields are lower than reported initially). Samples of all complexes were re-prepared in the course of putting these corrections together – the revised solvent content and yield of each of the samples is detailed below.

2. Due to point 1, everywhere in the paper and ESI file when we referred to 2·2H2O and 3·3.5H2O should now read [CoII2(LBrH-OBF3)2](BF4)2·4H2O (2′) and [CoII2(LClH-OBF3)2](BF4)2·2H2O (3′). Methanolysis of 2′ and 3′ presumably occurs to give the single crystals of 2·solvents and 3·solvents, the structures of which are correctly reported in the paper.

3. The PF6 complexes are only a very minor component of this paper (sentence in abstract p. 11749; synthesis discussion paragraph p. 11752; sentence in conclusion p. 11755; experimental sections starting at bottom p. 11756 and finishing p. 11757) but repeating these syntheses proved non-trivial so please disregard any comments made about those complexes, as they have never been made in analytically pure form.

Experimental

HL HBr . Elemental analysis: C 42.25, H 3.23, N 13.10, Calc. for [C15H14N4OBr2] (426.1 g mol−1): C 42.28, H 3.31, N 13.15.

HL BrH . Elemental analysis: C 42.20, H 3.10, N 12.95, Calc. for [C15H14N4OBr2] (426.1 g mol−1): C 42.28, H 3.31, N 13.15.

HL ClH . Elemental analysis: C 51.82, H 4.05, N 16.30, Calc. for [C15H14N4OCl2]·0.5H2O (346.2 g mol−1): C 52.04, H 4.37, N 16.18.

[Co II (HL HBr )(H 2 O) 2 ](BF 4 ) 2 ( 1′ ). (35 mg, 28%). Elemental analysis: C 25.77, H 2.50, N 7.82, Calc. for 1′ (694.7 g mol−1): C 25.93, H 2.61, N 8.07. TGA (5.026 mg, 80 °C for 180 min) found 5.48%; calculated weight loss for removal of 2H2O: 5.18%.

[CoII2(L BrH-OBF 3 ) 2 ](BF 4 ) 2 ·4H 2 O ( 2′ ). In air, solid HLBrH (53.5 mg, 0.126 mmol) was added to a pink solution of Co(BF4)2·6H2O (43 mg, 0.126 mmol) in MeOH (20 mL). The red solution was stirred for 6 hours, concentrated to 5 mL under reduced pressure and finally subjected to diethyl ether vapour diffusion. The resulting red powder was filtered off, air dried and subjected a second time to diethyl ether vapour diffusion into MeOH, to give [CoII2(LBrH-OBF3)2](BF4)2·4H2O (11 mg, 7%). Elemental analysis: C 27.06, H 2.69, N 8.68, Calc. for 2′ (tetrahydrate: 1349.3 g mol−1): C 26.70, H 2.54, N 8.30. TGA (3.353 mg, 80 °C for 60 min) found 5.74%; calculated weight loss for removal of 4H2O: 5.34%. Some single crystals of [CoII2(LBrH-BF2OMe)2](BF4)2·solvents (2·solvents) formed on recrystallisation of 2′ from MeOH/Et2O (methanolysis presumably converts ligand-O-BF3 to ligand-O-BF2OMe).

[CoII2(L ClH-OBF 3 ) 2 ](BF 4 ) 2 ·2H 2 O ( 3′ ). In air, solid HLClH (59 mg, 0.175 mmol) was added to a pink solution of Co(BF4)2·6H2O (59.6 mg, 0.175 mmol) in MeOH (20 mL). The red solution was stirred for 6 hours, concentrated to 5 mL under reduced pressure and finally subjected to diethyl ether vapour diffusion. The resulting red powder was filtered off, air dried and subjected a second time to diethyl ether vapour diffusion into MeOH, to give [CoII2(LClH-OBF3)2](BF4)2·2H2O (16 mg, 8%). Elemental analysis: C 31.49, H 3.09, N 10.29, Calc. for 3′ (dihydrate: 1135.5 g mol−1): C 31.73, H 2.66, N 9.87. TGA (3.226 mg, 80 °C for 180 min) found 2.96%; calculated weight loss for removal of 2H2O: 3.17%. Single crystals of [CoII2(LClH-BF2OMe)2](BF4)2·solvents (3·solvents) formed on recrystallisation of 3′ from MeOH/Et2O (methanolysis presumably converts ligand-O-BF3 to ligand-O-BF2OMe).

The Royal Society of Chemistry apologises for these errors and any consequent inconvenience to authors and readers.

Footnote

† Electronic supplementary information (ESI) available: Additional CSD search results; NMR spectra; possible ligand tautomers; IR spectra; microanalysis/TGA comparisons; X-ray crystallography tables; cyclic voltammetry results. CCDC reference numbers 1837189-1837191. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c9dt90173f
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