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Characterization of some synthetic Ru and Ir complexes by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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Author: Lou, X. · Buijtenen, J. van · Bastiaansen, J.J.A.M. · Waal, B.F.M. de · Langeveld, B.M.W. · Dongen, J.L.J. van
Publisher: Wiley
Institution: TNO Industrie en Techniek
Source:Journal of Mass Spectrometry, 5, 40, 654-660
Identifier: 238473
Keywords: Machines · Iridium complex · Matrix-assisted laser desorption/ionization mass spectrometry · Ruthenium complex · Acidity · Carboxylic acids · Complexation · Desorption · Laser applications · Reaction kinetics · Ruthenium compounds · Ligands · Sinapinic acid · Time-of-flight mass spectrometry (TOFMS) · Alpha cyano 4 hydroxycinnamic acid · Azo compound · Benzene derivative · Beta carboline · Bipyridine derivative · Dithranol · Gentisic acid · Hydroxyl group · Malononitrile · Nitro derivative · Pyridine derivative · Thymine derivative · Alkalinity · Analytic method


Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) was applied to the analysis of Ru(OCOCF 3)2(CO)(PPh3)2, Ru(OCOC 3F7)2(CO)(PPh3)2, Ir(tBuppy)3 and Ir(ppy)2(acac) complexes. A troublesome problem in the MALDI-TOFMS characterization of these metal complexes is the possible replacement of complex ligands by matrix. In this contribution, 10 matrices, ranging from acidic to basic, were investigated: α-cyano-4- hydroxycinnamic acid (CHCA), 2,5-dihydroxybenzoic acid (DHB), sinapinic acid (SA), dithranol, 2,4,6-trihydroxyactophenone (THAP), 6-azo-2-thiothymine (ATT), norharman, 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB), 4-nitroaniline (NA) and 2-amino-5-nitrophyridine (ANP). With most of the matrices, including the neutral and basic ones, matrix substitution of ligand could clearly be detected. Based on the experimental results, possible mechanisms of matrix substitution were discussed. It was demonstrated that the ligand exchange process might also occur through the gas-phase reactions initiated by laser shots. Among the matrices tested, DCTB was found to be the best one for the complexes that are prone to ligand exchange by matrix.