An unexpected lanthanum chloride carbonate hydrate: synthesis, crystal structure, vibrational spectra and thermal degradation of LaCl[CO3]·3H2O
-
Olaf Reckeweg
,
Falk Lissner
Abstract
Microcrystalline powders of LaCl[CO3]·3H2O were precipitated and isolated from stoichiometric aqueous solutions of LaCl3·7H2O and Na2[CO3]·10H2O. This confirmed the surprising emergence of corresponding single crystals during a reaction of equimolar aqueous solutions of LaCl3·7H2O and Na[N3] under ambient conditions by the uptake of atmospheric CO2. According to the X-ray structure analysis of colorless, transparent and rectangular single-crystals, LaCl[CO3]·3H2O adopts an orthorhombic structure, space group Pbca with the unit-cell parameters a=856.82(5), b=1598.57(9) and c=967.68(6) pm for Z=8. The tenfold coordination polyhedron around La3+ consists of two monodentate as well as two bidentate [CO3]2− anions together with three oxygen atoms from coordinating water molecules and one chloride anion. According to DSC/TG studies and X-ray powder diffraction, LaCl[CO3]·3H2O loses first its water and then carbon dioxide under thermal treatment up to 900°C to leave LaOCl behind. Vibrational infrared and Raman spectra confirmed the presence of H2O and [CO3]2− in LaCl[CO3]·3H2O and its stepwise degradation at elevated temperatures.
Dedicated to:
Professor Hans-Jürgen Meyer on the occasion of his 60th birthday.
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Articles in the same Issue
- Frontmatter
- In this Issue
- NQR, NMR, and X-ray crystal structure studies of [4-C2H5-C6H4NH3]2MBr4 (M=Zn, Cd)
- Ein ökonomisches Verfahren zur Aufarbeitung von Reaktionsgemischen bei Lewis-Säure-induzierten elektrophilen Aromatensubstitutionen
- Orthoamide und Iminiumsalze, XCIVa. Kondensationsreaktion von Orthoamiden von Alkincarbonsäuren mit 2-Methyl-5-phenacyl-1,3,4-thiadiazolen
- Highly effectual synthesis of 4,6-diarylpyrimidin-2(1H)-ones using N,N,N′,N′-tetramethylethylenediaminium-N,N′-disulfonic acid hydrogen sulfate as a dual-functional catalyst
- Efficient synthesis of pyrido[2,3-d]pyrimidine-7-carboxylic acids catalyzed by a TiO2/SiO2 nanocomposite in aqueous media at room temperature
- Synthesis, characterization, and antitumor activity of some novel S-functionalized benzo[d]thiazole-2-thiol derivatives; regioselective coupling to the –SH group
- A zinc(II) coordination polymer containing single- and double-stranded helical chains: synthesis, crystal structure, and thermal and luminescence properties
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