The DuPont powder challenge: The crystal structure of [C5NH6][Al3F10]-a cautionary tale

Chemistry of Materials

Volumn 11, Issue 9, 1999, Pages 2562-2567

  Harlow, Richard L ^a   Herron, Norman ^a   Li, Zhigang ^a   Vogt, Thomas ^a   Solovyov, Leonid ^a   Kirik, Sergei ^a  

^a DUPONT COMPANY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 6344282544     PISSN: 08974756     EISSN: None     Source Type: Journal    
DOI: 10.1021/cm990273x     Document Type: Article

References (7)

1. Herron, N.; Thorn, D. L.; Harlow, R. L.; Jones, G. A.; Parise, J. B.; Fernandez-Baca, J. A.; Vogt, T. Chem. Mater. 1995, 7, 75.
2. A powder sample of the compound was compressed into a deep flat plate holder and data were collected in high-resolution mode [Cox, D. E.; Toby, B. H.; Eddy, M. M.Aust. J. Phys. 1988, 41, 117] at the X7a beamline at the National Synchrotron Light Source, Brookhaven National Laboratory. The beamline was configured with a Si(111) monochromator and Ge(220) analyzer, a scintillation detector, and incident beam-defining slits of 8.0 mm by 1.5 mm. The wavelength, calibrated using a Si powder standard with a = 5.430 825 Å, was 0.848 78(3) Å. The data were collected in six scans covering a 2θ range from 4 to 40° with a step size of 0.02° and a total count time of 12 s per point. The sample was "rocked" by 0.5° at low angles increasing to 2.0° at the higher angles.
3. Herron, N.; Thorn, D. L.; Harlow, R. L.; Davidson, F. J. Am. Chem. Soc. 1993, 115, 3028.
4. The instrument is described in: Passell, L.; Bar-ziv, S.; Gardner, D. W.; Cox, D. E.; Axe, J. D. Mater. Sci. Forum 1991, 79, 475. The wavelength used was 1.8857 Å.
5. Le Bail, A. Laboratoire des Fluorures, CNRS UPRES-A 6010, Faculte des Sciences, Université du Maine, F-72085 Le Mans Cedex 9, France, personal communication.
6. Neels, A. Institute de Chemie de l'Universitéde Neuchatel, Avenue de Bellevaux 51, CH-2000, Neuchatel, Switzerland, personal communication.
7. Larsen, A. C.; Von Dreele, R. B. GSAS, Generalized Structure Analysis System; Los Alamos National Laboratory: Los Alamos, NM, 1986; LAUR 86-748.