International
Tables for
Crystallography
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 3.4, pp. 278-279

Section 3.4.4.6.1. Indexing using DICVOL06

A. Altomare,a* C. Cuocci,a A. Moliternia and R. Rizzia

aInstitute of Crystallography – CNR, Via Amendola 122/o, Bari, I-70126, Italy
Correspondence e-mail:  angela.altomare@ic.cnr.it

3.4.4.6.1. Indexing using DICVOL06

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The program DICVOL06, as implemented in the WinPLOTR/FULLPROF suite (Roisnel & Rodríquez-Carvajal, 2001[link]) and recently introduced into EXPO, was applied to two experimental diffraction patterns.

Example 1

Norbornene (Brunelli et al., 2001[link]). Published information: C7H10, monoclinic, a = 7.6063 (9), b = 8.6220 (1), c = 8.749 (1) Å, β = 97.24 (1)°, P21/c, experimental range 5–60° 2θ, λ = 0.85041 Å, RES = 1.0 Å (where RES is the data resolution), synchrotron data, indexed by Fzon (Visser, 1969[link]).

The 2θ values of the first 25 peaks, in the range 5–25°, were determined by WinPLOTR and supplied to DICVOL06. The first 20 peaks were used for searching for the solution. No plausible cell was found when assuming that no impurity was present and exploring all the systems (from cubic to triclinic). DICVOL06 was also unsuccessful when the non-default strategies of extended search and data correction for zero-point error were considered (by setting some flags to 1 in the input file). If it was supposed that two impurity lines might be present among the peaks (by setting the flag corresponding to the maximum number of accepted impurity/spurious lines to 2), DICVOL06 was able to find the following monoclinic cell: a = 8.7480 (36), b = 8.6313 (32), c = 7.6077 (26) Å, β = 97.201 (33)°, with two unindexed lines, M18 = 41.5, F18 = 125(0.0041, 35). The refinement of the cell by considering all the 25 lines gave a = 7.6087 (26), b = 8.6295 (30), c = 8.7459 (34) Å, β = 97.201 (34)°, which is very similar to the published one; 23 indexed lines, M20 = 30.1, F20 = 102.6(0.0048, 41). The presence of the two impurity lines has been ascribed by the authors to a small amount of hexagonal plastic phase.

Example 2

Cu(II)–Schiff base complex (Banerjee et al., 2002[link]). Published information: Cu(C15H12NO2)2, triclinic, a = 11.928 (4), b = 12.210 (5), c = 9.330 (5) Å, α = 102.54 (4), β = 111.16 (5), γ = 86.16 (4)°, [P \bar 1], experimental range 6–100° 2θ, λ = 1.54056 Å, RES = 1.22 Å, high-quality X-ray laboratory data, indexed by DICVOL91. The 2θ values of the first 30 peaks, in the range 6–25°, were determined by WinPLOTR and supplied to DICVOL06. The first 20 peaks were used for searching for the solution. If it was assumed that no impurity was present, no plausible cell was found down to the monoclinic system. When the triclinic system was explored, DICVOL06 suggested only one plausible solution: a = 12.2157 (73), b = 12.2031 (77), c = 9.3071 (41) Å, α = 65.798 (46), β = 102.572 (59), γ = 95.711 (61)°, with no unindexed lines, M20 = 27.0, F20 = 77.0(0.010, 26). The refinement of the cell considering all the 30 lines gave a = 12.2125 (65), b = 12.1989 (61), c = 9.3016 (32) Å, α = 65.826 (33), β = 102.569 (40), γ = 97.755 (44)°, no unindexed lines, M20 = 27.9, F20 = 72.8(0.0106, 26). For this,the corresponding conventional cell is a = 11.93313 (61), b = 12.2125 (65), c = 9.3016 (32) Å, α = 102.569 (40), β = 111.152 (33), γ = 86.151 (44)°, similar to the published one.

References

Banerjee, S., Mukherjee, A., Neumann, M. A. & Louër, D. (2002). Ab-initio structure determination of a Cu(II)-Schiff base complex from X-ray powder diffraction data. Acta Cryst. A58, c264.Google Scholar
Brunelli, M., Fitch, A. N., Jouanneaux, A. & Mora, A. J. (2001). Crystal and molecular structures of norbornene. Z. Kristallogr. 216, 51–55.Google Scholar
Roisnel, T. & Rodríquez-Carvajal, J. (2001). WinPLOTR: a windows tool for powder diffraction pattern analysis. Mater. Sci. Forum, 378–381, 118–123.Google Scholar
Visser, J. W. (1969). A fully automatic program for finding the unit cell from powder data. J. Appl. Cryst. 2, 89–95.Google Scholar








































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