Hostname: page-component-77c89778f8-fv566 Total loading time: 0 Render date: 2024-07-23T03:04:41.722Z Has data issue: false hasContentIssue false
  • English
  • Français

Revisiting the crystal structure of [Co(NH3)5Cl]Cl2 using synchrotron powder diffraction: to what extent single-crystal diffraction from 1960s got it right?

Published online by Cambridge University Press:  05 July 2017

S. Mohamud  and
S. Pagola
S. Mohamud
Affiliation:
Department of Physics, College of William and Mary, Williamsburg, Virginia 23185
S. Pagola*
Affiliation:
Department of Applied Science, College of William and Mary, Williamsburg, Virginia 23185
*
a)Author to whom correspondence should be addressed. Electronic mail: spagol@wm.edu
Get access Rights & Permissions [Opens in a new window]

Abstract

The crystal structure of the purpureo salt, [Co(NH3)5Cl]Cl2, first reported in 1963 and later revised in 1968 (in both cases from single-crystal diffraction) in the space group Pnma (No. 62), has been recently re-examined from synchrotron X-ray powder diffraction using direct methods and the software EXPO2013. The comparison of the Rietveld analysis results using the two published models and the atomic coordinates obtained from powders leads to an improved crystal structure description in the lower symmetry space group Pn21a (No. 33). As a result, the overall atom connectivity and crystal packing remain similar; however, the symmetry and internal geometry of the coordination complex are changed. The distortions from an idealized geometry in Pnma (No. 62) are likely because of energetically favorable hydrogen-bonding motifs in the crystal. The three models are compared, and their validity and limitations are discussed.

Keywords

X-ray powder diffractioncrystal structure solution from powderspurpureo salt
Type
Technical Articles
Information
Powder Diffraction , Volume 32 , Issue 3 , September 2017 , pp. 179 - 186
Check for updates
Copyright
Copyright © International Centre for Diffraction Data 2017 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Allen, F. H. (2002). “The Cambridge structural database: a quarter of a million crystal structures and rising,” Acta Crystallogr. B 58, 380–388.Google Scholar
Altomare, A., Cuocci, C., Giacovazzo, C., Moliterni, A., Rizzi, R., Corriero, N., and Falcicchio, A. (2013). “EXPO2013: a kit of tools for phasing crystal structures from powder data,” J. Appl. Crystallogr. 46(4), 1231–1235.CrossRefGoogle Scholar
Boultif, A. and Louër, D. (2004). “Powder pattern indexing with the dichotomy method,” J. Appl. Crystallogr. 37(5), 724–731.Google Scholar
Farrugia, L. (2012). “WinGX and ORTEP for windows: an update,” J. Appl. Crystallogr. 45(4), 849–854.Google Scholar
Larson, A. C. and vonDreele, R. B. (2004). General Structure Analysis System (GSAS) (Los Alamos National Laboratory Report 86–748). New Mexico, USA.Google Scholar
Le Bail, A. (2005). “Whole powder pattern decomposition methods and applications: a retrospection,” Powder Diffr. 20(4), 316–326.Google Scholar
Le Bail, A., Cranswick, L. M. D., Adil, K., Altomare, A., Avdeev, M., Cerny, R., Cuocci, C., Giacovazzo, C., Halasz, I., Lapidus, S. H., Louwen, J. N., Moliterni, A., Palatinus, L., Rizzi, R., Schilder, E. C., Stephens, P. W., Stone, K. H., and van Mechelen, J. (2009). “Third structure determination by powder diffractometry round robin (SDPDRR-3),” Powder Diffr. 24(3), 254–262.Google Scholar
Messmer, G. G. and Amma, E. L. (1968). “Redetermination of the crystal structure of chloropentamminecobalt(III) dichloride,” Acta Crystallogr. B 24, 417–422.Google Scholar
Scott, H. G. (1983). “The estimation of standard deviations in powder diffraction Rietveld refinements,” J. Appl. Crystallogr. 16, 159–163.Google Scholar
Sheldrick, G. M. (2008). “A short history of SHELX,” Acta Crystallogr. A 64, 112–122.Google Scholar
Shigeta, Y., Komiyama, Y., and Kuroya, H. (1963). “The crystal structure of purpureo salt, [Co(NH3)5Cl]Cl2 ,” Bull. Chem. Soc. Jpn. 36(9), 1159–1162.Google Scholar
Spek, A. L. (2002). “Single-crystal structure validation with the program PLATON,” J. Appl. Crystallogr. 36, 7–13.Google Scholar
Toby, B. H. (2006). “R factors in Rietveld analysis: how good is good enough?” Powder Diffr. 21(1), 67–70.CrossRefGoogle Scholar
Werner, P. E., Erikson, L., and Westdahl, M. (1985). “TREOR, a semi-exhaustive trial-and-error powder indexing program for all symmetries,” J. Appl. Crystallogr. 18, 367–370.Google Scholar
Supplementary material: File

Mohamud and Pagola supplementary material

Mohamud and Pagola supplementary material

Download Mohamud and Pagola supplementary material(File)
File 859.3 KB