Single-crystal structure refinement of hydrotalcite

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Marco E. Ciriotti
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Single-crystal structure refinement of hydrotalcite

Messaggio da Marco E. Ciriotti » mer 25 lug, 2018 15:47

Prossima pubblicazione.

Referenza:
▪ Zhitova, E.S., Krivovichev, S.V., Pekov, I.V., H.C. Greenwell, H.C. (2018): Crystal chemistry of natural layered double hydroxides. 5. Single-crystal structure refinement of hydrotalcite, [Mg6Al2(OH)16](CO3)(H2O)4. Mineralogical Magazine, 82, (in press).

Abstract:
Hydrotalcite, ideally [Mg6Al2(OH)16](CO3)(H2O)4, was studied in samples from 22 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-3m 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, 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 crystallizes in the P63/mmc space group, unit-cell parameters for two crystals are (data collection at room temperature 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. The paper reports the first single-crystal structure data on hydrotalcite. Hydrotalcite distribution in nature, diagnostic features, polytypism, interlayer topology and localization of M2+-M3+ cations within metal hydroxide layers are discussed.
Marco E. Ciriotti

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