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For an overview of the VenHCl, polymorph literature, their numbering as forms 1 -4, the characterization of sublimation form 5, and crystallization of polymorphs 1 and 2 for use in this study, see Roy, S.; Aitipamula, S.; Nangia, A. Cryst. Growth Des. 2005, 5, 2268.
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For an overview of the VenHCl, polymorph literature, their numbering as forms 1 -4, the characterization of sublimation form 5, and crystallization of polymorphs 1 and 2 for use in this study, see Roy, S.; Aitipamula, S.; Nangia, A. Cryst. Growth Des. 2005, 5, 2268.
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33947546096
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Crystal data: Form 6, C17H28NO2 +Cl, Mr 313.85, monoclinic,P21/n, T= 100(2) K, a, 5.887(10) Å b= 19.37(3) Å, c, 31.41(5) Å, β, 92.16(3)°, Z′, 2, Z, 8, V, 3579(10) Å3, μ (Mo-Kα) 0.218 mm-1, ρcalc, 1.165 g cm -3, R1,(I > 2σ(I, 0.1073. X-ray reflections were collected on Bruker SMART-APEX CCD diffrac-tometer (Mo-Kα radiation, λ, 0.71073 Å) with 10 s exposure time. Structures were solved and refined on F2 in SHELX-TL. H atoms were refined isotropically. The reported crystal structure data is the best solution we could derive from multiple experiments. Crystal data on polymorphs 1 and 2 are taken from the Cambridge Structural Database, CSD refcodes WO
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1(I > 2σ(I)) = 0. 068.
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23
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33947492237
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Geometry optimization was carried out using density functional theory (DFT) at the B3LYP/6-31.G (d,p) level in Gaussian 03, Revision B.05. http://www.gaussian.com.
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Geometry optimization was carried out using density functional theory (DFT) at the B3LYP/6-31.G (d,p) level in Gaussian 03, Revision B.05. http://www.gaussian.com.
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33947515797
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α radiation (λ = 1.54056 Å) with the generator power set at 40 kV and 40 mA. The sample was heated @ 10° min-1 and intensities were collected at regular T intervals in the 2θ range 5-50°. Full details of the VT-PXRD experiment are described in ref 13b.
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α radiation (λ = 1.54056 Å) with the generator power set at 40 kV and 40 mA. The sample was heated @ 10° min-1 and intensities were collected at regular T intervals in the 2θ range 5-50°. Full details of the VT-PXRD experiment are described in ref 13b.
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Simulation of the powder diffraction from the crystal structure and least-squares refinement of the experimental pattern was done in Powder Cell 2.3 ref 14b, The unit cell parameters were scaled to correct for the higher temperature of PXRD compared to single-crystal XRD measurement. The slight differences in peak intensity are due to the preferred orientation of the microcrystalline sample
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(a) Simulation of the powder diffraction from the crystal structure and least-squares refinement of the experimental pattern was done in Powder Cell 2.3 (ref 14b). The unit cell parameters were scaled to correct for the higher temperature of PXRD compared to single-crystal XRD measurement. The slight differences in peak intensity are due to the preferred orientation of the microcrystalline sample,
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