Seidlhofer, Beatrix, Antonova, Elena, Wang, Jing, Schinkel, Diana and Bensch, Wolfgang (2012) On the Complexity of Crystallization of Thioantimonates:In-situEnergy Dispersive X-ray Diffraction (EDXRD) Studies of the Solvothermal Formation of the Isostructural Thioantimonates [TM(tren)Sb4S7] (TM = Fe, Zn). Zeitschrift Fur Anorganische Und Allgemeine Chemie, 638 (15). pp. 2555-2564. DOI 10.1002/zaac.201200291.

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Abstract

The formation of the thioantimonates [M(tren)Sb4S7] (M = Fe, Zn; tren = tris(2‐aminoethyl)amine) has been studied with in‐situ energy dispersive X‐ray diffraction (EDXRD) under solvothermal conditions. Up to 60 % amine concentration the compound [Fe(tren)Sb4S7] coexists with an unknown crystalline material until the end of the reaction. In the concentration range 70–90 % amine the unknown compound and [Fe(tren)Sb4S7] are formed at the beginning of the reaction and when the unknown compound starts to disappear a new mixed‐valent thioantimonate [Fe(tren)FeSbS4] nucleates and crystallizes. Using a 100 % tren solution only [Fe(tren)FeSbS4] could be identified in the powder patterns. The analysis of the data collected under real conditions clearly shows a strong correlation between the disappearance of the unknown compound and the formation of the mixed‐valent thioantimonate. Evidences are presented that FeII/FeIII redox reactions play an important role for nucleation and crystal growth of a distinct iron‐containing thioantimonate. Because Zn2+ is not redox active the formation processes are different and no crystalline intermediate could be detected.

Document Type:	Article
Research affiliation:	Kiel University > Kiel Marine Science OceanRep > The Future Ocean - Cluster of Excellence Kiel University
Refereed:	Yes
Open Access Journal?:	No
Publisher:	American Medical Association
Projects:	Future Ocean
Date Deposited:	12 Jun 2018 10:34
Last Modified:	28 Mar 2019 13:15
URI:	https://oceanrep.geomar.de/id/eprint/43339

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