Mass spectrometric study of some zirconocene and hafnocene diadamantanolates

Grafov, Andriy; Koval, Lyudmila I.; Traldi, Pietro; Catinella, Silvia; Battiston, Giovanni A.; Zanella, P.

doi:10.1002/rcm.1290090915

Cited by 2 publications

(7 citation statements)

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“…MIKE spectra of its molecular ion [Cp 2 Hf(O2Ad)Cl] +· ( m/z 494) reveals three fragmentation pathways due to elimination of ligands. The most intense peak corresponds to the loss of chloro ligand producing a [Cp 2 Hf(O2Ad)] + ion ( m/z 459), already observed by us for the corresponding dialcoholato complex,8 and its further decomposition occurs similarly. Alternative elimination of the alcoholato moiety, responsible for appearance of the [Cp 2 HfCl] + ( m/z 343) fragment, is less significant.…”

Section: Resultssupporting

confidence: 53%

“…The most probable process under MIKE conditions corresponds to a complex one that comprises elimination of OC 3 H 4 and migration of the remaining hydrocarbon moiety to the metal, giving rise to [Cp 2 HfC 7 H 11 Cl] +· ( m/z 438). It is interesting to note that an analogous process was found also for the dialcoholato complex,8 but its probability was insignificant. The fragment in question undergoes further decomposition by two main channels.…”

Section: Resultsmentioning

confidence: 69%

“…A characteristic feature of mass spectra of the complexes under discussion is the presence of very intense peaks for their molecular ions, compared with those of similar dialcoholato derivatives 7,. 8 The relative intensities of these peaks decrease in the order O2Ad > O1Ad > OMAd ∼ OMNBM. The above indicates the quite high volatility and thermal stability of the complexes in question.…”

Section: Resultsmentioning

confidence: 98%

“…Within the context of our search for new prospective MOCVD precursors we synthesised3 a series of zirconocene and hafnocene derivatives with mono‐, bi‐ and tricyclic alcoholato ligands, studied their structures and properties,4,, 5 investigated their fragmentation in the gaseous phase,6–9 and obtained HfO 2 films 10. As a continuation of the above research it was of interest to study several mixed‐ligand metallocene complexes, in which only one chloro ligand was replaced by the alcoholato species.…”

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confidence: 99%

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Fragmentation study of mixed-ligand zirconocene and hafnocene alcoholates of the type Cp2M(OR)Cl

Grafov

Волков

Grafova

et al. 2000

Rapid Commun. Mass Spectrom.

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The electron ionisation mass spectrometric behaviour of a new series of hafnocene and zirconocene chloroalcoholates is discussed. These data are also compared with those of mass‐analysed ion kinetic energy spectrometry. With respect to dialcoholato complexes previously studied by us, the monochloro‐alcoholato species show rather high intensities in their molecular ion peaks, which reflects their higher volatility and sufficient stability in the vapour phase. Fragmentation patterns of the complexes in question give relevant information on their gas‐phase behaviour and also on the influence of the ligand structure on the decomposition pathways. The complexes in question appear to be promising precursors for metal‐organic chemical vapour deposition (MOCVD). Copyright © 2000 John Wiley & Sons, Ltd.

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Section: Resultssupporting

confidence: 53%

Section: Resultsmentioning

confidence: 69%

Section: Resultsmentioning

confidence: 98%

mentioning

confidence: 99%

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Fragmentation study of mixed-ligand zirconocene and hafnocene alcoholates of the type Cp2M(OR)Cl

Grafov

Волков

Grafova

et al. 2000

Rapid Commun. Mass Spectrom.

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“…In further decomposition steps the bicyclic moiety can be readily eliminated giving rise to a relatively small number of framework decomposition products (especially in the case of borneolates). Taking into consideration our previous studies of zirconocene and hafnocene adamantanolates, 7 mentholates, 4 derivatives containing bicyclo[3. …”

Section: Discussionmentioning

confidence: 99%

Fragmentation study of zirconocene and hafnocene dialcoholates containing trimethylbicyclo[2.2.1]heptane moieties

Grafov

Traldi

Grafova

et al. 1999

Rapid Commun. Mass Spectrom.

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The electron ionisation mass spectrometric behaviour of a new series of hafnocene and zirconocene dialcoholates is discussed. Deprotonated moieties of borneol and fenchyl alcohol were used as '-ligands. These data are also compared to those of mass-analysed ion kinetic energy spectroscopy of the molecular ions. Fragmentation patterns of the complexes in question give relevant information on their gas-phase behaviour and also on the influence of the ligand structure on the decomposition pathways. The complexes in question appear to be promising metal-organic chemical vapour decomposition precursors. Copyright # 1999 John Wiley & Sons, Ltd. Received 13 November 1998; Revised 2 December 1998; Accepted 3 December 1998 Recently the method of metal-organic chemical vapour deposition (CVD) has attracted much attention as a promising tool for obtaining new functional materials possessing valuable properties. A choice of suitable volatile and thermally stable organometallic precursors for the above technique is very important, 1 hence the particular efforts of many researchers has been concentrated on the correlation between the structure of the precursor and composition of final products to be obtained. From this point of view, mass spectrometry is one of the most informative methods. Its combination with mass-analysed ion kinetic energy (MIKE) spectroscopy in particular gives the possibility to reveal a fragmentation pattern of a compound under investigation which reasonably corresponds to that realised upon thermal decomposition. In turn, such information enables us to control the CVD processes and to obtain functional films with predictable composition.Oxides and carbides of zirconium and hafnium are well known as the best refractory coatings, and thus a search for volatile CVD precursors containing these metals, for example their co-ordination compounds, is always worthwhile. Traditionally, this role has been played by Zr or Hf tetraalkyls, tetraalcoholates, b-diketonates and, to a lesser extent, by dichlorides of zirconocene or hafnocene.2 The latter are of special interest to us due to a possibility to enhance considerably their volatility and thermal stability by substitution of hard donor chloro ligands by '-ligands containing voluminous organic frameworks, able to shield effectively the centre of coordination from interactions with neighbouring molecules. 5,6 ) and tricyclic (adamantanols 7 ) alcoholato ligands. Our mass spectrometric investigations show that the compounds in question are interesting and promising CVD precursors, in particular the metallocene derivatives of bicyclo[2.2.1]heptanols. The present paper is devoted to the investigation of the mass spectrometric behaviour of some complexes containing substituted trimethylbicyclo[2.2.1]-heptane moieties. EXPERIMENTALAll complexes were synthesised and purified by procedures developed by us and described in detail elsewhere.3,8 For convenience we use the following acronyms for the alcohols: HOBL for borneol (1,7,7-trimethylbicyclo[2.2.1]-heptan-2-ol)...

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Mass spectrometric study of some zirconocene and hafnocene diadamantanolates

Cited by 2 publications

References 2 publications

Fragmentation study of mixed-ligand zirconocene and hafnocene alcoholates of the type Cp2M(OR)Cl

Fragmentation study of mixed-ligand zirconocene and hafnocene alcoholates of the type Cp2M(OR)Cl

Fragmentation study of zirconocene and hafnocene dialcoholates containing trimethylbicyclo[2.2.1]heptane moieties

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