4.6 Article

Solid-phase synthesis of protonated nitrogen-containing heterocyclic compounds with the boron cluster anions starting from [Eu(H2O)9]2[B10Cl10]3: Synthesis, structure, and thermal properties of (HL)2[B10Cl10] (L=7-amino-4-methylcoumarin or 1-ethyl-2-(4-methoxyphenyl) azobenzimidazole)

期刊

JOURNAL OF SOLID STATE CHEMISTRY
卷 302, 期 -, 页码 -

出版社

ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jssc.2021.122413

关键词

Decachloro-closo-decaborate anion; X-ray diffraction; Thermal properties; Azaheterocyclic ligands

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The paper introduces a new method for synthesizing salts of a perchlorinated derivative of the decahydro-closodecaborate anion with neutral N-containing organic bases using a previously prepared europium precursor. The influence of reaction conditions on the composition and structure of the final products was analyzed, and the thermal properties of the obtained salts and ligand were studied in air.
The paper proposes a new method for the synthesis of salts of a perchlorinated derivative of the decahydro-closodecaborate anion with neutral N-containing organic bases L-1 and L-2 starting from previously prepared europium precursor [Eu(H2O)(9)](2)[B10Cl10](3). Compound [Eu(H2O)(9)](2)[B10Cl10](3) was first synthesized and characterized by elemental analysis, X-ray powder diffraction, IR spectroscopy and its thermal properties were studied by TGA. The protonation of organic bases L was carried out in the solid phase in the presence of precursor [Eu(H2O)(9)](2)[B10Cl10](3). For comparison, the reaction was carried out in solution: in the CH3CN/CF3COOH system and in an aqueous solution of (H3O)(2)[B10Cl10] with pronounced acidic properties. The influence of reaction conditions on the composition and structure of the final products was analyzed. Salts of the composition (HL)(2)[B10Cl10] (L is 1-ethyl-2-(4-methoxyphenyl)azobenzimidazole (L1) and 7-amino-4-methylcoumarin (L-2)) and (HL2)(H9O4) [B10Cl10] were synthesized and characterized by X-ray diffraction. The thermal properties of the obtained salts and ligand L1 (C16H16N4O) were studied in air in the temperature range 20-600 degrees C.

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