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Crystals of 5 and 9 have been obtained from the n-heptane solution. The diffraction experiments were performed for 0.63×0.33×0.20 mm yellow crystal of 5 and for 0.41×0.21×0.10 mm yellow crystal of 9. The X-ray data were collected at 291(2) K with an Oxford Sapphire CCD diffractometer using MoKα radiation λ =0.71073 Å by ω-2θ method. The numerical absorption correction was applied (CrysAlis171 package of programs, Oxford Diffraction, 2000) with the maximum and minimum transmissions of 0.5524 and 0.2203 for 5 and 0.7465 and 0.3503 for 9
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Crystals of 5 and 9 have been obtained from the n-heptane solution. The diffraction experiments were performed for 0.63×0.33×0.20 mm yellow crystal of 5 and for 0.41×0.21×0.10 mm yellow crystal of 9. The X-ray data were collected at 291(2) K with an Oxford Sapphire CCD diffractometer using MoKα radiation λ =0.71073 Å by ω-2θ method. The numerical absorption correction was applied (CrysAlis171 package of programs, Oxford Diffraction, 2000) with the maximum and minimum transmissions of 0.5524 and 0.2203 for 5 and 0.7465 and 0.3503 for 9. The structure of 5 was solved in the triclinic P1 space group and structure of 9 was determined in the orthorhombic P2(1)2(1)2 space group. The structures were solved with direct methods and refined with the full-matrix leastsquares method on F2 with the use of SHELX-97 program package[13]. The hydrogen atoms have been located from the difference electron density maps and constrained during refinement. The absolute structure has been determined with the Flack method [14], the Flack x value being -0.008(13) for 5 and -0.014(11) for 9. The structural data have been deposited with Cambridge Crystallographic Data Centre, the CCDC numbers 689256 and 689255, respectively.
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