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<p>The development of metal-based drugs capable of releasing NO in a controlled manner is of great interest due to their biological responses, including anticancer activities. To this end, the compounds <i>cis-</i>[Ru(NO)Cl(cyclen)]X<sub>2</sub> (X = Cl<sup>−</sup> or ClO<sub>4</sub><sup>−</sup>) and <i>cis</i>-[RuCl<sub>2</sub>(cyclen)]Cl were synthesized using efficient ultrasound-assisted methods. The nitrosyl complex was fully characterized by FTIR, UV-Vis spectroscopy, NMR, and single crystal XRD. Its reactivity was investigated through electrochemical and photochemical studies. The complex was found to release NO upon photolysis at 365&#xa0;nm, with an apparent quantum yield of 0.204&#xa0;mol/Einstein. The kinetics of ligand release upon reduction revealed a two-step process: a rapid chloride release (<i>k</i><sub><i>1</i></sub> = 10.1&#xa0;s<sup>− 1</sup>) followed by a much slower NO release (<i>k</i><sub>2</sub> = 3.0 × 10<sup>− 4</sup> s<sup>− 1</sup> at 25&#xa0;°C). Electrochemical investigations supported a mechanism involving the formation of the aqua-nitrosyl intermediate, <i>cis</i>-[Ru(NO)(H<sub>2</sub>O)(cyclen)]<sup>2+</sup>, and elucidated the parallel pathways leading to the final Ru(II)-aqua species. These experiments enhance our understanding of the nitrosyl complex reactivity towards reduction and photochemical processes, highlighting its potential as a controlled NO-releasing metallodrug.</p>

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Ultrasound-mediated synthesis of Ruthenium(II) nitrosyl cyclen complex: crystal structure, electrochemical and photochemical behavior

  • 期刊论文

  • 发表日期：

    2026年2月4日

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  • Tamires Mariel Muniz Milhazes,
  • Gabriela Andrade dos Santos,
  • Maiara O. Passos,
  • Camila B. Pinto,
  • Javier A. Ellena,
  • Alzir A. Batista,
  • Soraia Teixeira Brandão,
  • Roberto Santana da Silva,
  • Kleber Queiroz Ferreira

摘要

The development of metal-based drugs capable of releasing NO in a controlled manner is of great interest due to their biological responses, including anticancer activities. To this end, the compounds cis-[Ru(NO)Cl(cyclen)]X2 (X = Cl− or ClO4−) and cis-[RuCl2(cyclen)]Cl were synthesized using efficient ultrasound-assisted methods. The nitrosyl complex was fully characterized by FTIR, UV-Vis spectroscopy, NMR, and single crystal XRD. Its reactivity was investigated through electrochemical and photochemical studies. The complex was found to release NO upon photolysis at 365 nm, with an apparent quantum yield of 0.204 mol/Einstein. The kinetics of ligand release upon reduction revealed a two-step process: a rapid chloride release (k1 = 10.1 s− 1) followed by a much slower NO release (k2 = 3.0 × 10− 4 s− 1 at 25 °C). Electrochemical investigations supported a mechanism involving the formation of the aqua-nitrosyl intermediate, cis-[Ru(NO)(H2O)(cyclen)]2+, and elucidated the parallel pathways leading to the final Ru(II)-aqua species. These experiments enhance our understanding of the nitrosyl complex reactivity towards reduction and photochemical processes, highlighting its potential as a controlled NO-releasing metallodrug.