Three-Dimensional Structure Determination of N-(p-Tolyl)-dodecylsulfonamide from Powder Diffraction Data and Validation of Structure Using Solid-State NMR Spectroscopy

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• 作者：Manju Rajeswaran ; Thomas N. Blanton ; Nicholas Zumbulyadis ; David J. Giesen ; Carlota Conesa-Moratilla ; Scott T. Misture ; Peter W. Stephens ; and Ashfia Huq
• 刊名：Journal of the American Chemical Society
• 出版年：2002
• 出版时间：December 4, 2002
• 年：2002
• 卷：124
• 期：48
• 页码：14450 - 14459
• 全文大小：538K
• 年卷期：v.124,no.48(December 4, 2002)
• ISSN：1520-5126

文摘

The three-dimensional structure, conformation, and packing of molecules in the solid state arecrucial components used in the optimization of many technologically useful materials properties. Single-crystal X-ray diffraction is the traditional and most effective method of determining 3-D structures in thesolid state. Obtaining single crystals that are sufficiently large and free of imperfections is often laborious,time-consuming, and, occasionally, impossible. The feasibility of an integrated approach to the determinationand verification of a complete three-dimensional structure for a medium-sized organic molecule withoutusing single crystals is demonstrated for the case of an organic stabilizer compound N-(p-tolyl)-dodecylsulfonamide. The approach uses a combination of powder XRD data, several computationalpackages involving Monte Carlo simulations and ab initio quantum mechanical calculations, and experimentalsolid-state NMR chemical shifts. Structure elucidation of N-(p-tolyl)-dodecylsulfonamide revealed that theBravais lattice is monoclinic, with cell dimensions of a = 38.773 Å, b = 5.507 Å, c = 9.509 Å, and rs/beta2.gif" BORDER=0 ALIGN="middle"> =86.35, and a space group of P21/c.