Ionothermal synthesis of β-NH4AlF4 and the determination by single crystal X-ray diffraction of its room temperature and low temperature phases

被引:22
作者
Parnham, Emily R. [1 ]
Slawin, Alex M. Z. [1 ]
Morris, Russell E. [1 ]
机构
[1] Univ St Andrews, E Chem Sch Chem, St Andrews KY16 9ST, Fife, Scotland
基金
英国工程与自然科学研究理事会;
关键词
Ionothermal; beta-NH4AlF4; X-ray diffraction; 1-ethyl-3-methylimidazolium hexafluorophosphate;
D O I
10.1016/j.jssc.2006.09.024
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
beta-NH4AlF4 has been synthesised ionothermally using 1-ethyl-3-methylimidazolium hexafluorophosphate as solvent and template provider. beta-NH4AlF4 crystals were produced which were suitable for single crystal X-ray diffraction analysis. A phase transition occurs between room temperature (298 K) and low temperature (93 K) data collections. At 298 K the space group = I4/mcm (no. 140), alpha = 11.642(5), c = 12.661(5) angstrom, Z = 2 (10NH(4)AlF(4)), wR(F-2) = 0.1278, R(F) = 0.0453. At 93 K the space group = P4(2)/ncm (no. 138), alpha = 11.616(3), c = 12.677(3) angstrom, Z = 2 (10NH(4)AlF(4)), wR(F-2) = 0.1387, R(F) = 0.0443. The single crystal X-ray diffraction study of beta-NH4AlF4 shows the presence of two different polymorphs at low and room temperature, indicative of a phase transition. The [AlF4/2F2](-) layers are undisturbed except for a small tilting of the AlF6 octahedra in the c-axis direction. (c) 2006 Elsevier Inc. All rights reserved.
引用
收藏
页码:49 / 53
页数:5
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