Scandium(iii) 1,1,1-trifluorohexane-2,4-dionate complex: Synthesis, structure, and thermal properties

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Abstract

A new scandium(III) 1,1,1-trifluorohexane-2,4-dionate complex [Sc(5Htfac)3] was synthesized, purified, and characterized by elemental analysis, NMR spectroscopy, and mass spectrometry. Its structure was determined at 150 K by X-ray diffraction analysis (CCDC No. 2433044). The complex has a molecular structure in which the bidentate cyclic ligands are arranged according to the os-isomer. Shortened H…F interactions were identified in the structure. The thermal properties were studied by TGA and DSC, and the fusion temperature (309.3 ± 0.5 K), enthalpy (ΔfusH°(Tfus) = 36.0 ± 1.4 kJ mol–1), and entropy (ΔfusS°(Tfus) = = 116.5 ± 4.5 J mol–1 K–1) of fusion were determined. The temperature dependence of the saturated vapor pressure was measured by the flow method (343–433 K) and the static method with a membrane null manometer (410–470 K). On this basis, the thermodynamic characteristics of evaporation at average and standard temperatures were calculated (ΔvapH°(298.15 K) = 100.2 ± 1.3 kJ mol–1, ΔvapS°(298.15 K) = = 201.8 ± 2.8 J mol–1 K–1). From these data, the sublimation parameters of the complex were obtained (ΔsubH°(298.15 K) = 135.3 ± 1.9 kJ mol–1, ΔsubS°(298.15 K) = 315.3 ± 5.4 J mol–1 K–1). The structure and thermal properties of [Sc(5HTfac)3] were compared with those of two scandium(III) β-diketonates bearing methyl and tert-butyl substituents in the ligand.

About the authors

A. V. Sartakova

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Email: a.sartakova@alumni.nsu.ru
Novosibirsk, Russia

S. V. Sysoev

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Novosibirsk, Russia

A. M. Makarenko

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Novosibirsk, Russia

N. V. Kurat’eva

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Novosibirsk, Russia

D. P. Pishchur

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Novosibirsk, Russia

K. V. Zherikova

Nikolaev Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences

Novosibirsk, Russia

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