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Chromium chains as polydentate fluoride ligands for lanthanides

Chemical Communications
The Royal Society of Chemistry
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Microsoft Word - Cr12Ln4 Supplementary Information.docx Supplementary Information Chromium Chains as Polydentate Fluoride Ligands for Lanthanides Andrew McRobbie,a Asad R. Sarwar,a Steven Yeninas,b Harriott Nowell,c Michael L. Baker,a,d David Allan,c Marshall Luban,b Christopher A. Muryn,a Robin G. Pritchard,a Ruslan Prozorov,b* Grigore A. Timco,a Floriana Tuna,a George F. S. Whiteheada and Richard E. P. Winpenny Synthesis The reagents were from Aldrich and used as received. [(Et2NH2)3Cr6F11(O2CtBu)10]2 and [(nPr2NH2)3Cr6F11(O2CtBu)10]2 were prepared according S.T. Ochsenbein et al.Chem. Eur. J. 2008, 14, 5144 – 5158. The [Ln(O2CtBu)3(HO2CtBu)3]2 complexes were prepared as reported in T.A. Zoan et al. J. Alloys & Comp., 1995, 225, 396-399. Compound 3: [Cr6CeF7(O2CtBu)14 (THF)2] [(nPr2NH2)3Cr6F11(O2CtBu)10]2 (2.0g, 0.54mmol), Gd(O2CtBu)3(HO2CtBu)3]2 (2.0g, 1.33mmol) and pivalic acid (2.0g, 19.58mmol) were dissolved in toluene (100mL) and DMSO (2 g) and refluxed with stirring for 1.5h at 125ºC. Once the reaction mixture had been allowed to cool to room temperature the solvent was removed under reduced pressure and to MeCN (30 ml) was added to the residue and stirred for 0.5h. The solid was collected by filtration, washed with further MeCN and dried in air. Column chromatography on silica gel with 1:20 EtOAc-Toluene as the eluent was used to purify the collected solid. The title compound was collected with first fraction in a very low yield. Crystals suitable for an X-ray structure study were obtained by crystallization from a mixture of THF-MeCN. Elemental analysis calculated (%) for C78H142CeCr6F7O30 : C 43.82, H 6.69, N 0.00; found (%) C 42.09, H 6.73, N 0.00. Compound 4: [Et2NH2)2Cr12Gd2F18(O2CtBu)26], [Gd(O2CtBu)3(HO2CtBu)3]2 (0.5 g, 0.326 mmol ), pivalic acid (1.5 g, 14.69 mmol ), DMSO (1.0 g) and [(Et2NH2)3Cr6F11(O2CtBu)10]2 (1.5 g , 0.427 mmol ) were stirred at room temperature with THF (35 ml) for 15 min, then MeCN ( 20

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