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Preparation and characterization of 1: Anhydrous PrCh (1.6 g, 6.5 mmol) was added to a stirred THF solution (100 ml) of in situ prepared Li 2(COT″, 12 mL (19.2 mmol) of a 1.6 M n-butyllithium solution in n-hexane and 2.35 g (9.4 mmol) of C8H6(SiMe 3)2-1,4) at room temperature. The reaction mixture was stirred for 2 weeks and refluxed for another 1 h. Solvents were evaporated under vacuum, and the residue was extracted with boiling toluene (ca. 40 mL, Concentration and cooling to 3 °C afforded 1 as orange-yellow needles (2.5 g, 83, which were suitable for X-ray crystallography. Anal. Calc for C 92H160Cl8Li2O2Pr 6S12 (2778.25, C 39.77, H 5.80. Found: C 39.91, H 5.88, The crystals lose toluene of crystallization upon thorough drying under vacuum, 1H NMR (C6D6, 400.1 MHz, 20 °C, 6.42-5.58 br m, C
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34748923992
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int= 0.0855). Final Rl = 0.0577, wR2 = 0.1426 (all data). CCDC-641044.
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int= 0.0855). Final Rl = 0.0577, wR2 = 0.1426 (all data). CCDC-641044.
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