Synthesis, LIFDI Mass Spectrometry and Reactivity of Triacyl‐Germenolates

Drusgala, Manfred; Linden, Mathias H.; Knoechl, Andreas; Torvisco, Ana; Fischer, Roland; Linden, H. Bernhard; Haas, Michael

doi:10.1002/ejic.202100441

Cited by 8 publications

(10 citation statements)

References 24 publications

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“…Especially taking into account the complexity the aforementioned aspects, a promising alternative to EI-MS is liquid injection field desorption/ionization mass spectrometry (LIFDI-MS). [20][21][22][23] As a special derivative of the field desorption (FD) method for the reliable mass spectral analysis of labile, thermally unstable and nonpolar complexes, LIFDI provides an easy-to-access platform for the determination of analytes by MS that are additionally reactive toward the ambient and thus inaccessible for EI-MS without taking special precautions. In LIFDI, a metal wire with microscopic whiskers, the so-called activated emitter, is exposed to the dissolved analyte (1 mg min −1 ) which is transferred by a thin glass injection capillary under vacuum.…”

Section: Introductionmentioning

confidence: 99%

Liquid injection field desorption/ionization as a powerful tool to characterize volatile, labile, and reactive metal–organic complexes

Boysen

Devi

2022

Eur J Mass Spectrom (Chichester)

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Electron ionization mass spectrometry (EI-MS) is often used to characterize volatile and thermally stable organometallic complexes relevant for chemical vapor deposition (CVD) processes. However, this method has limitations for thermally unstable and labile organometallic complexes. In this context, EI-MS is not the preferred method of choice for characterizing such compounds. With three different representative organometallic complexes based on the transition metals yttrium, iridium, and silver, relevant as precursors for CVD of different materials, the significance of liquid injection field desorption/ionization mass spectrometry (LIFDI-MS) as an important precursor characterization tool is exemplified. The precursors are not only reactive toward ambient air, but also thermally labile especially in the case of iridium and silver complexes. As a promising alternative, LIFDI-MS is used to overcome the limitations of EI-MS. For the first time, these complexes were successfully analyzed using LIFDI-MS. The comparison between EI-MS and LIFDI-MS highlights that LIFDI-MS is superior for the mass spectrometric analysis of sensitive and labile complexes. In terms of precursor characterization, LIFDI-MS can be fully exploited to gain valuable insights into the decomposition mechanisms and identifying the nuclearity of organometallic precursors used for CVD applications.

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Section: Introductionmentioning

confidence: 99%

Liquid injection field desorption/ionization as a powerful tool to characterize volatile, labile, and reactive metal–organic complexes

Boysen

Devi

2022

Eur J Mass Spectrom (Chichester)

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“…Direct Approach toward 4a−c P21̅ n and the unit cell contains four molecules. In close analogy to other structurally characterized germenolates, [6][7][8][9]12,13 the central Ge atoms are pyramidal and have elongated Ge−C single bonds. Noteworthy is an interesting structural feature in the structure of 5.…”

Section: Electron-transfer Reactions Of Other Alkali Metals (Methods A)mentioning

confidence: 65%

“…Historically speaking, the synthesis and characterization of heavier group 14 (HG 14) enolates were mainly triggered by fundamental investigations in the field of main group chemistry. − Recently, we could demonstrate that HG 14 triacylenolates (M = Ge and Sn) represent innovative building blocks for the formation of high-performance free-radical photoinitiators. − To synthesize these new HG 14 triacylenolates, we established two pathways. The first methodology uses a potassium-induced single-electron-transfer (SET) approach starting from the respective tetraacyl derivatives.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of New Counterion-Substituted Triacylgermenolates and Investigation of Selected Metal–Metal Exchange Reactions

et al. 2022

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The synthetic process to obtain triacylgermenolates with alternated counterions by single-electron-transfer reactions or by a direct approach is described. The formation of these derivatives was confirmed by NMR spectroscopy and UV–vis spectroscopy. Moreover, metal–metal exchange reactions of potassium-substituted triacylgermenolate 2a with MgBr 2 , ZnCl 2 , and HgCl 2 are presented. Additionally, 2a was reacted with n Bu 4 NBr, which led to the formation of ammonia-substituted triacylgermenolate 8 . Furthermore, we reacted 2a with HCl/Et 2 O to obtain triacylgermane 9 . Subsequently, we investigated the reaction of 9 with t Bu 2 Zn and t Bu 2 Hg. NMR spectroscopy, single-crystal X-ray crystallography, and UV–vis spectroscopy are employed for analysis of structural properties.

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“…In order to adjust the absorption wavelength, a series of multi-acyl-substituted germanes have been prepared as photoinitiators. [78][79][80][81][82][83][84][85][86][87] However, in photoinduced organic reactions, only single-acyl-group-substituted germanes have been used as substrates.…”

Section: Acylgermanesmentioning

confidence: 99%