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  Modular Ion Mobility Calibrants for Organometallic Anions Based on Tetraorganylborate Salts

Auth, T., Grabarics, M., Schlangen, M., Pagel, K., & Koszinowski, K. (2021). Modular Ion Mobility Calibrants for Organometallic Anions Based on Tetraorganylborate Salts. Analytical Chemistry, 93(28), 9797-9807. doi:10.1021/acs.analchem.1c01333.

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Modular Ion Mobility Calibrants for Organometallic Anions Based on Tetraorganylborate Salts (2021).pdf (beliebiger Volltext), 6MB
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Auth, Thomas1, Autor
Grabarics, Márkó2, 3, Autor           
Schlangen, Maria4, Autor
Pagel, Kevin2, 3, Autor           
Koszinowski, Konrad1, Autor
Affiliations:
1Institut für Organische und Biomolekulare Chemie, Universität Göttingen, Tammannstraße 2, Göttingen 37077, Germany, ou_persistent22              
2Institut für Chemie und Biochemie, Freie Universität Berlin, Arnimallee 22, Berlin 14195, Germany, ou_persistent22              
3Molecular Physics, Fritz Haber Institute, Max Planck Society, ou_634545              
4Institut für Chemie, Technische Universität Berlin, Straße des 17. Juni 115, Berlin 10623, Germany, ou_persistent22              

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 Zusammenfassung: Organometallics are widely used in catalysis and synthesis. Their analysis relies heavily on mass spectrometric methods, among which traveling-wave ion mobility spectrometry (TWIMS) has gained increasing importance. Collision cross sections (CCS) obtainable by TWIMS significantly aid the structural characterization of ions in the gas phase, but for organometallics, their accuracy has been limited by the lack of appropriate calibrants. Here, we propose tetraorganylborates and their alkali-metal bound oligomers [Mn–1(BR4)n] (M = Li, Na, K, Rb, Cs; R = aryl, Et; n = 1–6) as calibrants for electrospray ionization (ESI) TWIMS. These species chemically resemble typical organometallics and readily form upon negative-ion mode ESI of solutions of alkali-metal tetraorganylborates. By combining different tetraorganylborate salts, we have generated a large number of anions in a modular manner and determined their CCS values by drift-tube ion mobility spectrometry (DTIMS) (DTCCSHe = 81–585, DTCCSN2 = 130–704 Å2). In proof-of-concept experiments, we then applied these DTCCS values to the calibration of a TWIMS instrument and analyzed phenylcuprate and argentate anions, [Lin–1MnPh2n] and [MnPhn+1] (M = Cu, Ag), as prototypical reactive organometallics. The TWCCSN2 values derived from TWIMS measurements are in excellent agreement with those determined by DTIMS (<2% relative difference), demonstrating the effectiveness of the proposed calibration scheme. Moreover, we used theoretical methods to predict the structures and CCS values of the anions considered. These predictions are in good agreement with the experimental results and give further insight into the trends governing the assembly of tetraorganylborate, cuprate, and argentate oligomers.

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Sprache(n): eng - English
 Datum: 2021-03-282021-06-222021-07-062021-07-20
 Publikationsstatus: Erschienen
 Seiten: 11
 Ort, Verlag, Ausgabe: -
 Inhaltsverzeichnis: -
 Art der Begutachtung: Expertenbegutachtung
 Identifikatoren: DOI: 10.1021/acs.analchem.1c01333
 Art des Abschluß: -

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Titel: Analytical Chemistry
  Kurztitel : Anal. Chem.
Genre der Quelle: Zeitschrift
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Ort, Verlag, Ausgabe: Washington, D.C. : American Chemical Society
Seiten: 11 Band / Heft: 93 (28) Artikelnummer: - Start- / Endseite: 9797 - 9807 Identifikator: ISSN: 0003-2700
CoNE: https://pure.mpg.de/cone/journals/resource/111032812862552