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Single-molecule magnetism in cyclopentadienyl-dysprosium chlorides

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Journal
Chemical Communications
1359-7345
Publisher
The Royal Society of Chemistry
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Abstract

Microsoft Word - Cp2DyCl Chem Comm ESI.doc 1 Chemical Communications Supplementary Information for: Single-molecule magnetism in cyclopentadienyl-dysprosium chlorides Scott A. Sulway,a Richard A. Layfield,a* Floriana Tuna,a,c Wolfgang Wernsdorferb and Richard E. P. Winpennya,c* a School of Chemistry, The University of Manchester, Oxford Road, Manchester, M13 9PL, U.K. E-mail: [email protected] bInstitut Néel, CNRS and Université J. Fourier, BP 166, 25, Avenue des Martyrs, F-38042, Grenoble, France. c The Photon Science Institute, The University of Manchester, Oxford Road, Manchester, M13 9PL, U.K. E-mail: [email protected] Electronic Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2011 2 General experimental considerations All synthetic manipulations were performed using standard Schlenk techniques. Toluene was degassed and dried by refluxing over sodium-potassium alloy under nitrogen. X-ray diffraction data on 1a, 1b and 2 were collected on an OXFORD Diffraction XCaliber2 CCD diffractometer using MoK radiation. SQUID measurements were carried out on polycrystalline samples of 1 and 2 by enclosing the sample in O-ring-sealed Kel-F capsules. The capsules were transferred to sample holders in a glovebox, transported to the SQUID magnetometer in a sealed Schlenk tube, and then rapidly transferred to the helium-purged sample space of the magnetometer. Corrections for diamagnetism were made using Pascal’s constants. Synthesis of 1a and 1b. A freshly prepared solution of sodium cyclopentadienide (37 mmol) in thf (60 mL) was added to a stirred suspension of anhydrous dysprosium(III) chloride (5.00 g, 18 mmol) in thf (100 mL) at 0°C. The mixture was refluxed for 16 hours and the solvent then evaporated under reduced pressure, producing a pale yellow solid. Sublimation of the yellow solid (10-3 mbar/180C) resulted in the formation of ye

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