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Synthesis, Crystal Structure, and Thermal Decomposition of La(CH3SO3)3 · 2 H2O

✍ Scribed by Mathias S. Wickleder

Publisher
John Wiley and Sons
Year
2001
Tongue
German
Weight
172 KB
Volume
627
Category
Article
ISSN
0372-7874

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✦ Synopsis

La(CH 3 SO 3 ) 3 ´2 H 2 O was prepared by the reaction of La 2 O 3 with CH 3 SO 3 H. According to the X-ray single crystal determination, the compound crystallizes with triclinic symmetry (P 1, Z = 2, a = 524.99( 8), b = 1015.3(2), c = 1298.0(2) pm, a = 98.62(2)°, b = 91.12(2)°, c = 104.61(2)°, R all = 0.0405) and contains ninefold coordinate La 3+ ions. The coordination polyhedra are tricapped trigonal prisms which are connected by CH 3 SO 3 ± ions to double chains. These are linked via hydrogen bonding only. The thermal decomposition of La(CH 3 SO 3 ) 3 ´2 H 2 O was investigated by means of temperature dependent X-ray powder diffraction and DSC/TG/EGA methods. The compound dehydrates in a first step around 120 °C to give the anhydrous methanesulfonate which decomposes finally yielding La 2 O 2 S 2 . According to the powder diffraction results the anhydrous methane sulfonate La(CH 3 SO 3 ) 3 crystallizes with a hexagonal structure (P6 3 /m, a = 998.26(6), c = 597.97(6) pm) which has been found for the respective perchlorate, hydrogensulfate, and amidosulfate previously. Synthese, Kristallstruktur und thermisches Verhalten von La(CH 3 SO 3 ) 3 ´2 H 2 O Inhaltsu È bersicht. La(CH 3 SO 3 ) 3 ´2 H 2 O wurde durch Umsetzung von La 2 O 3 mit CH 3 SO 3 H erhalten. Nach den Ergebnissen der Ro È ntgenstrukturanalyse kristallisiert die Verbindung triklin (P 1, Z = 2, a = 524,99(8), b = 1015,3(2), c = 1298,0(2) pm, a = 98,62(2)°, b = 91,12(2)°, c = 104,61(2)°, R all = 0,0405) und entha È lt neunfach koordinierte La 3+ -Ionen. Die Koordinationspolyeder ko È nnen als dreifach bekappte trigonale Prismen gesehen werden, die u È ber CH 3 SO 3 ± -Ionen zu Doppelketten verbunden sind, welche ihrerseits nur von Wasserstoffbru È ckenbindungen zusammengehalten werden.

Das thermische Verhalten von La(CH 3 SO 3 ) 3 ´2 H 2 O wurde mit Hilfe von DSC/TG/EGA-Messungen und temperaturabha È ngiger Pulverdiffraktometrie untersucht. Danach dehydratisiert die Verbindung zuna È chst bei etwa 120 °C zu La(CH 3 SO 3 ) 3 , welches sich schlieûlich unter Bildung von La 2 O 2 S 2 zersetzt. Die wasserfreie Verbindung kristallisiert nach Ausweis der Pulveruntersuchungen hexagonal (P6 3 /m, a = 998,26(6), c = 597,97(6) pm) und ist isotyp zu La(ClO 4 ) 3 , La(HSO 4 ) 3 und La(NH 2 SO 3 ) 3 .

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