Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory
Abstract
:1. Introduction
2. Results and Discussion
3. Materials and Methods
4. Conclusion
Supplementary Materials
Acknowledgments
Author Contributions
Conflicts of Interest
References
- Kabekkodu, S. PDF-4+ 2016 (Database); International Centre for Diffraction Data: Newtown Square, PA, USA, 2016. [Google Scholar]
- Van de Streek, J.; Neumann, M.A. Validation of molecular crystal structures from powder diffraction data with dispersion-corrected density functional theory (DFT-D). Acta. Cryst. Sect. B Struct. Sci. Cryst. Eng. Mater. 2014, 70, 1020–1032. [Google Scholar]
- Macrae, C.F.; Bruno, I.J.; Chisholm, J.A.; Edington, P.R.; McCabe, P.; Pidcock, E.; Rodriguez-Monge, L.; Taylor, R.; van de Streek, J.; Wood, P.A. Mercury CSD 2.0-new features for the visualization and investigation of crystal structures. J. Appl. Crystallogr. 2008, 41, 466–470. [Google Scholar] [CrossRef]
- Wavefunction, Inc. Spartan ’14 Version 1.1.0; Wavefunction Inc.: Irvine, CA, USA, 2013. [Google Scholar]
- Dassault Systèmes. Materials Studio 8.0; BIOVIA: San Diego, CA, USA, 2014. [Google Scholar]
- Hirshfeld, F.L. Bonded-atom fragments for describing molecular charge densities. Theor. Chem. Acta. 1977, 44, 129–138. [Google Scholar] [CrossRef]
- McKinnon, J.J.; Spackman, M.A.; Mitchell, A.S. Novel tools for visualizing and exploring intermolecular interactions in molecular crystals. Acta. Cryst. Sect. B 2004, 60, 627–668. [Google Scholar] [CrossRef] [PubMed]
- Spackman, M.A.; Jayatilaka, D. Hirshfeld surface analysis. Cryst. Eng. Comm. 2009, 11, 19–32. [Google Scholar] [CrossRef]
- Wolff, S.K.; Grimwood, D.J.; McKinnon, M.J.; Turner, M.J.; Jayatilaka, D.; Spackman, M.A. Crystal Explorer Version 3.1; University of Western Australia: Crawley, Australia, 2012. [Google Scholar]
- Bravais, A. Etudes Cristallographiques; Gauthier Villars: Paris, France, 1866. [Google Scholar]
- Friedel, G. Etudes sur la loi de Bravais. Bull. Soc. Fr. Mineral. 1907, 30, 326–455. [Google Scholar]
- Donnay, J.D.H.; Harker, D. A new law of crystal morphology extending the law of Bravais. Am. Mineral. 1938, 22, 446–467. [Google Scholar]
- Lee, P.L.; Shu, D.; Ramanathan, M.; Preissner, C.; Wang, J.; Beno, M.A.; Von Dreele, R.B.; Ribaud, L.; Kurtz, C.; Antao, S.M.; et al. A twelve-analyzer detector system for high-resolution powder diffraction. J. Synch. Rad. 2008, 15, 427–432. [Google Scholar] [CrossRef] [PubMed]
- Wang, J.; Toby, B.H.; Lee, P.L.; Ribaud, L.; Antao, S.M.; Kurtz, C.; Ramanathan, M.; Von Dreele, R.B.; Beno, M.A. A dedicated powder diffraction beamline at the Advanced Photon Source: Commissioning and early operational results. Rev. Sci. Inst. 2008, 79, 085105. [Google Scholar] [CrossRef] [PubMed]
- MDI. Jade 9.5; Materials Data. Inc.: Livermore, CA, USA, 2010. [Google Scholar]
- Groom, C.R.; Bruno, I.J.; Lightfoot, M.P.; Ward, S.C. The Cambridge Structural Database. Acta Crystallogr. Sect. B Struct. Sci. Cryst. Eng. Mater. 2016, 72, 171–179. [Google Scholar] [CrossRef] [PubMed]
- O’Boyle, N.; Banck, M.; James, C.A.; Morley, C.; Vandermeersch Hutchison, G.R. Open Babel: An open chemical toolbox. J. Chem. Informatics 2011, 3, 33. [Google Scholar] [CrossRef] [PubMed]
- Favre-Nicolin, V.; Černý, R. FOX, ‘free objects for crystallography’: A modular approach to ab initio structure determination from powder diffraction. J. Appl. Crystallogr. 2002, 35, 734–743. [Google Scholar] [CrossRef]
- Larson, A.C.; Von Dreele, R.B. General Structure Analysis System, (GSAS); Los Alamos National Laboratory Report LAUR: Los Alamos, NM, USA, 2004. [Google Scholar]
- Dovesi, R.; Orlando, R.; Civalleri, B.; Roetti, C.; Saunders, V.R.; Zicovich-Wilson, C.M. CRYSTAL: A computational tool for the ab initio study of the electronic properties of crystals. Zeit. Kristallogr. 2005, 220, 571–573. [Google Scholar] [CrossRef]
- Dovesi, R.; Orlando, R.; Erba, A.; Zicovich-Wilson, C.M.; Civalleri, B.; Casassa, S.; Maschio, L.; Ferrabone, M.; De La Pierre, M.; D-Arco, P.; et al. A program for the ab initio investigation of crystalline solids. Int. J. Quantum Chem. 2014, 114, 1287–1317. [Google Scholar] [CrossRef]
- Gatti, C.; Saunders, V.R.; Roetti, C. Crystal-field effects on the topological properties of the electron-density in molecular crystals—The case of urea. J. Chem. Phys. 1994, 101, 10686–10696. [Google Scholar] [CrossRef]
- Toby, B.H. EXPGUI, a graphical user interface for GSAS. J. Appl. Crystallogr. 2001, 34, 210–213. [Google Scholar] [CrossRef]
- Sykes, R.A.; McCabe, P.; Allen, F.H.; Battle, G.M.; Bruno, I.J.; Wood, P.A. New software for statistical analysis of Cambridge Structural Database data. J. Appl. Crystallogr. 2011, 44, 882–886. [Google Scholar] [CrossRef] [PubMed]
- Bruno, I.J.; Cole, J.C.; Kessler, M.; Luo, J.; Motherwell, W.D.S.; Purkis, L.H.; Smith, B.R.; Taylor, R.; Cooper, R.I.; Harris, S.E.; et al. Retrieval of crystallographically-derived molecular geometry information. J. Chem. Inf. Sci. 2004, 44, 2133–2144. [Google Scholar] [CrossRef] [PubMed]
- Thompson, P.; Cox, D.E.; Hastings, J.B. Rietveld refinement of Debye-Scherrer synchrotron X-ray data from Al2O3. J. Appl. Crystallogr. 1987, 20, 79–83. [Google Scholar] [CrossRef]
- Finger, L.W.; Cox, D.E.; Jephcoat, A.P. A correction for powder diffraction peak asymmetry due to axial divergence. J. Appl. Crystallogr. 1994, 27, 892–900. [Google Scholar] [CrossRef]
- Stephens, P.W. Phenomenological model of anisotropic peak broadening in powder diffraction. J. Appl. Crystallogr. 1999, 32, 281–289. [Google Scholar] [CrossRef]
H-Bond | D-H, Å | H···A, Å | D···A, Å | D-H···A, ° | Overlap, e | E, kcal/mol |
---|---|---|---|---|---|---|
O18-H39···O20 | 0.986 | 1.943 | 2.927 | 174.9 | 0.061 | 13.5 |
O20-H40-O18 | 0.976 | 1.952 | 2.902 | 163.6 | 0.043 | 11.3 |
© 2017 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/).
Share and Cite
Kaduk, J.A.; Gindhart, A.M.; Blanton, T.N. Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory. Crystals 2017, 7, 218. https://doi.org/10.3390/cryst7070218
Kaduk JA, Gindhart AM, Blanton TN. Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory. Crystals. 2017; 7(7):218. https://doi.org/10.3390/cryst7070218
Chicago/Turabian StyleKaduk, James A., Amy M. Gindhart, and Thomas N. Blanton. 2017. "Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory" Crystals 7, no. 7: 218. https://doi.org/10.3390/cryst7070218