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6
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33845548948
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8
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0036602127
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0037159789
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62649175270
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X-Ray Crystal structure determinations: A colorless prismatic crystal of C21H27NOBr2 having an approximate dimension of 0.4 x 0.4 x 0.4 mm grown from hexane was used for the data collection of a Rigaku AFC 7R diffractometer with graphic monochromated Cu-Koα radiation, r, 1.54178 Å) and rotating anode generator. Crystal data of 5d, M, 469.26; orthorhombic, space group P212121, 19, Z, 4 with a, 10.979(2) Å, b, 19.261(4) Å, c, 10.289(1) Å, V, 2175.8(6) Å3, and Dcale, 1.432g/cm3. All calculations were performed using the teXsan program. The structure was solved by direct methods and expanded using Fourier techniques. The final R- and Rw-factors after full-matrix least-squares refinement were 0.043 and 0.040, respectively, based on 1475 observed reflections (I>3.00σI
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w-factors after full-matrix least-squares refinement were 0.043 and 0.040, respectively, based on 1475 observed reflections (I>3.00σ(I)).
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