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Crystal chemistry of natural layered double hydroxides. 5. Single-crystal structure refinement of hydrotalcite, [Mg6Al2(OH)16](CO3)(H2O)4

Published online by Cambridge University Press:  25 July 2018

Elena S. Zhitova*
Department of Crystallography, Institute of Earth Sciences, St. Petersburg State University, St. Petersburg, Russia
Sergey V. Krivovichev
Department of Crystallography, Institute of Earth Sciences, St. Petersburg State University, St. Petersburg, Russia Nanomaterials Research Centre, Kola Science Centre, Russian Academy of Sciences, Apatity, Russia
Igor Pekov
Department of Mineralogy, Faculty of Geology, Moscow State University, Moscow, Russia
H. Christopher Greenwell
Department of Earth Sciences, Durham University, Durham, UK, DH1 3LE
*Author for correspondence: Elena S. Zhitova, Email:


Hydrotalcite, ideally [Mg6Al2(OH)16](CO3)(H2O)4, was studied in samples from Dypingdal, Snarum, Norway (3R and 2H), Zelentsovskaya pit (2H) and Praskovie–Evgenievskaya pit (2H) (both Southern Urals, Russia), Talnakh, Siberia, Russia (3R), Khibiny, Kola, Russia (3R), and St. Lawrence, New York, USA (3R and 2H). Two polytypes, 3R and 2H (both ‘classical’), were confirmed on the basis of single-crystal and powder X-ray diffraction data. Their chemical composition was studied by electron-microprobe analysis, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The crystal structure of hydrotalcite-3R was solved by direct methods in the space group R$ {\bar 3} $m on three crystals (two data collections at 290 K and one at 120 K). The unit-cell parameters are as follows (290/290/120 K): a = 3.0728(9)/3.0626(3)/3.0617(4), c = 23.326(9)/23.313(3)/23.203(3) Å and V = 190.7(1)/189.37(4)/188.36(4) Å3. The crystal structures were refined on the basis of 304/150/101 reflections to R1 = 0.075/0.041/0.038. Hydrotalcite-2H crystallises in the P63/mmc space group; unit-cell parameters for two crystals are (data collection at 290 K and 93 K): a = 3.046(1)/3.0521(9), c = 15.447(6)/15.439(4) Å, V = 124.39(8)/124.55(8) Å3. The crystal structures were refined on the basis of 160/142 reflections to R1 = 0.077/0.059. This paper reports the first single-crystal structure data on hydrotalcite. Hydrotalcite distribution in Nature, diagnostic features, polytypism, interlayer topology and localisation of M2+M3+ cations within metal hydroxide layers are discussed.

Copyright © Mineralogical Society of Great Britain and Ireland 2018 

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Associate Editor: Anthony Kampf


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