Structure and Thermal Properties of Volatile Iridium(I) Complexes with Cyclooctadiene-1,5 and β-Ketohydrazonate Ligands

K. I. Karakovskaya, E. S. Vikulova, T. S. Sukhikh, I. Yu Ilyin, N. B. Morozova

Research output: Contribution to journalArticlepeer-review

Abstract

Within the search for novel promising volatile precursors for the atomic layer deposition new mixed-ligand complexes of iridium(I) with β-ketohydrazones are obtained: [Ir(cod)(dmht)] 1 and [Ir(cod)(dmha)] 2 (cod = cyclooctadiene-1,5, dmht = CF3C(O)CHC(NN(CH3)2)CH3, dmha = CH3C(O)CHC(NN(CH3)2)CH3). The compounds are characterized by the elemental analysis, IR and NMR spectroscopy, and their structures are determined by single crystal X-ray diffraction. In the complex molecules there is a distorted square coordination core IrNOC2′ (C′ is the center of the C=C bond in the cod ligand). The Ir-O, Ir-N bond lengths and Ir-C′ distances are in narrow ranges of 2.027(5)–2.039(3) Å, 2.046(6)–2.074(3) Å, and 1.982(5)–2.017(3) Å respectively. The crystal packing of 1 is of the layered type. Weak pair interactions γC-H…F are observed between the layers. The molecules of 2 form columns packed in the square motif. Shortened intermolecular contacts are not revealed in this structure. The shortest Ir…Ir distances are 5.357 A and 6.420 A in 1 and 2 structures respectively. The synthesized complexes are capable of a quantitative transition to the vapor phase (100–120 °C, 0.05 Torr) and are characterized by relatively low melting points (105 °C and 121 °C for 1 and 2 respectively). The structure and thermal properties (thermogravimetry data) of β-ketohydrazonate complexes [Ir(cod)(L)] are compared with those of the related compounds containing β-diketonata and β-ketoiminate ligands.

Original languageEnglish
Pages (from-to)109-118
Number of pages10
JournalJournal of Structural Chemistry
Volume61
Issue number1
DOIs
Publication statusPublished - 1 Jan 2020

Keywords

  • iridium(I)
  • single crystal X-ray diffraction analysis
  • thermal analysis
  • volatile precursor
  • β-ketohydrazonate
  • THIN-FILMS
  • OXIDE
  • beta-ketohydrazonate
  • CHEMISTRY
  • WATER OXIDATION
  • ATOMIC LAYER DEPOSITION
  • PRECURSORS

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