References
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- Wasserman , H. , Aubrey , N. and Zimmerman , H. 1953 . J. Am. Chem. Soc. , 75
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- Compound 3 crystallized in the centrosymmetric, monoclinic space group P 21/n. The unit ceil parameters were determined to be a - 6.567(2) Å, b = 10.143(3) Å, c = 16.231(5) Å, and 6–101. 98(2)° by least squares fitting to the positions of 25 independent reflections in the range 23° ⩽ 2θ ⩾ 26°. This unit cell contained four asymmetric units of molecular formula C8H14Br2O2 in a volume of 1048.6(8) Å3, which produces a calculated density of 1.9 g/cm3. The structure was solved on a Nicolet R3m/E crystallographic system using the θ:2θ scan routine and graphite monochromated MoKα radiation (δ = 0.71069 Å) at approximately −100°C. After Lorentz and polarization corrections, the structure was solved by the SHELXTL 5.1 programs. All non -hydrogen atoms were refined anisotropically. The approximate location of all hydrogen atoms was determined by Fourier difference syntheses. Crystallographic parameters for compound 3 have been deposited with the Cambridge Crystallographic Database.