Just Published in Inorganic Chemistry

Authors: Tristan Zach, Florian Geyer, Benjamin Kiendl, Jan Mößeler, Olivier Nguyen, Thomas Schmidpeter, Patrick Schuster, Christoph Nagel, and Ulrich Schatzschneider*

Abstract: In a combinatorial approach, a family of ruthenium(II) azido complexes [Ru(N₃)(N∧N)(terpy)]PF₆ with terpy = 2,2′:6′,2″-terpyridine and N∧N as a bidentate chelator derived from 2,2′-biypridine and its 4,4′-disubstituted derivatives, 2,2′-bipyrimidine, and 1,10-phenanthroline were reacted with different internal and terminal alkynes to give access to a total of 7 × 7 = 49 triazolato complexes in a room-temperature catalyst-free iClick reaction. The reactants were mixed in a repurposed high-performance liquid chromatography (HPLC) autosampler, and the reaction progress was monitored by direct injection into an electrospray mass spectrometer. The ratio of the peak intensities of [Ru(N₃)(N∧N)(terpy)]⁺ and [Ru(triazolato)(N∧N)(terpy)]⁺ was converted to a colored heat map for facile visual inspection of the conversion ratio. By automated multiple injections of the reaction mixture in fixed time intervals and plotting peak intensities over reaction time, pseudo-first-order rate constants were easily determined. Finally, nonoverlapping isotope patterns of the azido starting materials and triazolato products enabled multiplexed parallel determination of rate constants for four different ruthenium(II) azido complexes from a single sample vial, thereby reducing experiment time by 75%.

Link: https://pubs.acs.org/doi/10.1021/acs.inorgchem.2c03377