Hydrogen Bonding of OOH Group in Crystalline Adducts of Organic Hydroperoxides with Cage Tertiary Amines, Their N-Oxides, and a Phosphine Oxide: A Combined X-ray Crystallography and DFT Study

  • Ivan A. Buldashov
  • , Pavel A. Egorov
  • , Alexey A. Mikhaylov
  • , Elena A. Mel’nik
  • , Tatiana A. Tripol’skaya
  • , Ovadia Lev
  • , Petr V. Prikhodchenko*
  • *Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

Abstract

Cocrystallization with appropriate organic molecules has been known as an effective and practical strategy for stabilization of organic hydroperoxides─useful oxidants, free-radical polymerization initiators, and emerging pharmaceuticals. In this paper, two peroxosolvates (H2O2·HMTA (1), 0.843H2O2·0.157H2O·DABCO N-oxide (2)) and 11 adducts of organic hydroperoxides (2tBuOOH·DABCO (3), 2CmOOH·DABCO (4), 2tBuOOH·HMTA (5), 3tBuOOH·DABCO N-oxide (6), CmOOH·Ph3PO (7), Cy(OOH)2·DABCO N-oxide (8), Cy(OOH)2·DABCO N-oxide·0.5C6H6 (9), [Cy(OOH)O]2·HMTA N-oxide (10), [Cy(OOH)O]2·DABCO N-oxide (11), [Cy(OOH)O]2·2DABCO N-oxide·2CHCl3 (12), [Cy(OOH)O]2·Ph3PO (13)) were structurally characterized for the first time, providing the relationships with the nature of components. The energetic superiority of O–H···O–N+ and O–H···O═P over O–H···N hydrogen bonds (EHB = 30.5–69.3 kJ mol–1) was against the lower basicity of amine N-oxides and Ph3PO over amine coformers. This was computationally attributed to the nearly 3-fold increase of partial atomic charges in the former hydrogen bond acceptors, in light of the interaction electrostatic nature. Nine compounds were synthesized according to the proposed facile approach and investigated by FTIR and Raman spectroscopy, thermal analysis, and powder XRD. Thermal stability of the cocrystals was found to be improved by the utilization of heavy coformers and less volatile hydroperoxides, rather than being correlated with hydrogen bond energy.

Original languageEnglish
Pages (from-to)10397-10412
Number of pages16
JournalCrystal Growth and Design
Volume25
Issue number24
DOIs
StatePublished - 17 Dec 2025

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© 2025 American Chemical Society

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