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(b) The authors have deposited atomic coordinates for this structure with the Cambridge Crystallographic Data Centre. The coordinates can be obtained, on request, from the Director, Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge, CB2 1EZ, UK.
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Barton deoxygenation of the xanthate derivative and Wolf-Kishner reduction of the tosylhydrazone derivative failed. Attempts to prepare the tosylate or iodide derivative of the corresponding primary alcohol, as a prelude to reduction, were also unsuccessful.
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3 and BINAP were purchased from Aldrich Chemical Co. High-resolution mass spectra were measured on a MicroMass Analytical 7070E spectrometer (EI or CI-isobutane); uncertainty (s) in mass measurements is 1.0 millimass unit (molecular weight < 400) or 1.5 millimass units (molecular weight 400-1000). Other general experimental details have been described: Deng, W.; Overman, L. E. J. Am. Chem. Soc. 1994, 116, 11241.
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