Mechanochemical conglomerate formation by ball milling - or not?
Abstract
Inspired by a study reporting on the zinc oxide-induced mechanochemical conglomerate formation of racemic amino acids, we investigated the reaction behavior of the analogous 19F-labeled DL-valine. Solid-state NMR spectroscopy under magic-angle spinning (MAS) conditions was employed as the central analytical technique to analyze the reaction products. In contrast to our expectation, no conglomerate formation occurred, and in the presence of ZnO and methanol a polymeric complex with one zinc and two fluorinated valine molecules was formed in a vibrational ball mill. Repeating these experiments with non-fluorinated valine led to a rather unusual and unique tetranuclear species with an overall composition of Zn4(D-Val)4(L-Val)4 as determined by single-crystal analysis and solid-state NMR. The latter complex was also formed when an equimolar ratio of the two enantiopure valine phases was combined in the ball mill with ZnO and methanol. The use of Resonant Acoustic Mixing (RAM) led to the same complex, but the efficiency of its formation varied significantly depending on the reaction conditions.
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BibTeX
@misc{moos2026mechanochemical,
title = {{Mechanochemical conglomerate formation by ball milling - or not?}},
author = {Sven Moos and Pascal Trommelschläger and Tobias Krückel and Calogero Quaranta and Niklas Aengenvoort and Fabio Manzoni and Jas S. Ward and Kathrin Rübartsch and Mirijam Zobel and Manu Lahtinen and Kari Rissanen and Carsten Bolm and Thomas Wiegand},
howpublished = {ChemRxiv},
year = {2026},
month = oct,
doi = {10.26434/chemrxiv.15009741/v1},
url = {https://chemrxiv.org/doi/full/10.26434/chemrxiv.15009741/v1},
note = {CC BY},
}
RIS
TY - UNPB
TI - Mechanochemical conglomerate formation by ball milling - or not?
AU - Sven Moos
AU - Pascal Trommelschläger
AU - Tobias Krückel
AU - Calogero Quaranta
AU - Niklas Aengenvoort
AU - Fabio Manzoni
AU - Jas S. Ward
AU - Kathrin Rübartsch
AU - Mirijam Zobel
AU - Manu Lahtinen
AU - Kari Rissanen
AU - Carsten Bolm
AU - Thomas Wiegand
PY - 2026
DA - 2026/10/01
PB - ChemRxiv
DO - 10.26434/chemrxiv.15009741/v1
UR - https://chemrxiv.org/doi/full/10.26434/chemrxiv.15009741/v1
AB - Inspired by a study reporting on the zinc oxide-induced mechanochemical conglomerate formation of racemic amino acids, we investigated the reaction behavior of the analogous 19F-labeled DL-valine. Solid-state NMR spectroscopy under magic-angle spinning (MAS) conditions was employed as the central analytical technique to analyze the reaction products. In contrast to our expectation, no conglomerate formation occurred, and in the presence of ZnO and methanol a polymeric complex with one zinc and two fluorinated valine molecules was formed in a vibrational ball mill. Repeating these experiments with non-fluorinated valine led to a rather unusual and unique tetranuclear species with an overall composition of Zn4(D-Val)4(L-Val)4 as determined by single-crystal analysis and solid-state NMR. The latter complex was also formed when an equimolar ratio of the two enantiopure valine phases was combined in the ball mill with ZnO and methanol. The use of Resonant Acoustic Mixing (RAM) led to the same complex, but the efficiency of its formation varied significantly depending on the reaction conditions.
ER -