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<p>In a search for volatile fluorinated compounds of potassium and rubidium, new complexes of the corresponding pivaloyltrifluoroacetonates (Ptac) with 18-crown-6 ether, [K(18C6)(Ptac)] (<b>I</b>) and [Rb(18C6)(Ptac)] (<b>II</b>), were synthesized. The compounds were characterized by elemental analysis, IR spectroscopy, and X-ray fluorescence analysis, and their structures were studied by single-crystal X-ray diffraction (SCXRD) in the range of 100–400 K (CCDC nos. 2429226–2429232 (<b>I</b>), 2429233–2429239 (<b>II</b>)). The complexes are isostructural and have an molecular mononuclear structure, with M…H and M…C contacts involving the <i>tert-</i>butyl group between fragments, forming chains. The thermal expansion tensors are elongated along this direction. X-ray diffraction analysis showed that the rubidium cation in such a complex can complete its coordination sphere with a solvent molecule (chloroform, CCDC no. 2429240 (<b>IIs</b>)). For <b>I</b>, <b>II</b>, and <b>IIs</b>, Hirshfeld surface were analyzed and a search for pseudoperiodicity in the crystal packings was carried out using the translational sublattice method. Thermogravimetric analysis showed that, unlike the initial pivaloyltrifluoroacetonates, complexes <b>I</b> and <b>II</b> are volatile and promising for testing in gas-phase processes of thin-film material deposition.</p>

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Complexes of Pivaloyltrifluoroacetonates of Potassium and Rubidium with 18-Crown-6 Ether: Synthesis, Structure, Thermal Properties

  • 期刊论文

  • 发表日期：

    2025年7月1日

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  • D. V. Kochelakov,
  • E. S. Vikulova

摘要

In a search for volatile fluorinated compounds of potassium and rubidium, new complexes of the corresponding pivaloyltrifluoroacetonates (Ptac) with 18-crown-6 ether, [K(18C6)(Ptac)] (I) and [Rb(18C6)(Ptac)] (II), were synthesized. The compounds were characterized by elemental analysis, IR spectroscopy, and X-ray fluorescence analysis, and their structures were studied by single-crystal X-ray diffraction (SCXRD) in the range of 100–400 K (CCDC nos. 2429226–2429232 (I), 2429233–2429239 (II)). The complexes are isostructural and have an molecular mononuclear structure, with M…H and M…C contacts involving the tert-butyl group between fragments, forming chains. The thermal expansion tensors are elongated along this direction. X-ray diffraction analysis showed that the rubidium cation in such a complex can complete its coordination sphere with a solvent molecule (chloroform, CCDC no. 2429240 (IIs)). For I, II, and IIs, Hirshfeld surface were analyzed and a search for pseudoperiodicity in the crystal packings was carried out using the translational sublattice method. Thermogravimetric analysis showed that, unlike the initial pivaloyltrifluoroacetonates, complexes I and II are volatile and promising for testing in gas-phase processes of thin-film material deposition.