| CrystEngComm, 2003, 5 | |
Additions and corrections Solventless isomerisation reactions: A crystallographic and thermomicroscopic investigation of some six coordinate RuCl2L2L′2 complexes |
Owen P. M. Horwood, David G. Billing, Demetrius C. Levendis, Florence M. Nareetsile and Neil J. Coville
CrystEngComm, 2003, 5, DOI: 10.1039/b313093b. Amendment published 15th October 2004
Please replace Table 1 from the paper with Table 1 given below:
| Table 1 Heating experiments of ttt-RuCl2(t-BuNC)2(PPh3)2 single crystals | ||||
| Expt. No. | Temperature/ºC | Duration | Observations | |
| 1a | 180d | 4–5 min | At 179–180 ºC crystals started
to darken rapidly. At expt. end: crystals had clear (yellow) and dark (black)
regions. Crystal morphology unchanged. XRDf: Crystal structure of ttt-isomer (starting material) solved. NMRg: 65% ttt-isomer, 35% cct-isomer. |
|
| 2b | 180e | 11 h | At expt. end: crystals totally darkened.
Crystal morphology unchanged. XRDf: microcrystalline powder rings. NMRg: 56% ttt-isomer, 44% cct-isomer. |
|
| 3b | 180e | 30 h | At expt. end: crystals totally darkened.
Crystal morphology unchanged. XRDf: microcrystalline powder rings. |
|
| 4a | 180d | 48 min | At 165–170 ºC the initially
yellow crystals turned ligh orange in colour. At 180 ºC crystals started to
darken rapidly, then more slowly. At expt. end: crystals almost completely
darkened. Crystal morphology unchanged. XRDf: microcrystalline powder rings. |
|
| 5a | 165d | 1 h | At expt. end: crystals not darkened
(remained yellow). Crystal morphology unchanged. XRDf: Crystal structure of ttt-isomer (starting material) solved. |
|
| 6c | 165d | 5 h | At 155 ºC the initially yellow
crystals turned light orange in colour. At 160 ºC crystals started to
darken slowly. At expt. end: crystals totally darkened. Crystal morphology
unchanged. XRDf: microcrystalline powder rings. |
|
| 7c | 155d | 4 h | After 20 min crystals started to darken
slowly. At expt. end: crystals had clear (yellow) and dark (black) regions.
Crystal morphology unchanged. XRDf: Feint powder rings detected. Crystal structure of ttt-isomer (starting material) solved. NMRg: 67% ttt-isomer, 33% cct-isomer. |
|
| a Heating plate cell used. b Shortened NMR tube used, flushed with N2 gas, immersed in oil bath. c Heated gas stream cell used. d Heating rate to experiment temperature: 2.5 ºC min–1. e Heating rate to experiment temperature: 10 ºC min–1. f XRD behaviour of selected crystals tested on single-crystal diffractometer. g Minimum of 3–4 crystals dissolved in CDCl3, 400 MHz spectrometer, ttt- and cct-isomer Me resonance (1H NMR data) compared. | ||||
The Royal Society of Chemistry apologises for these errors and any consequent inconvenience to authors and readers.