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Novel bis(β-diketonato)diorganotin(IV) derivatives containing bulky 4-acyl-5-pyrazolonato ligands : Influence of the steric hindrance of the acyl moiety on the solid state structures of tin complexes and their behaviour in solution
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Caruso, F. (Francesco), Di Nicola, Corrado, Hanna, John V., Marchetti, F. (Fabio), Pettinari, Claudio, Pettinari, Riccardo, Rossi, Miriam, Rees, Gregory J., Skelton, Brian W. and White, Allan H. (2011) Novel bis(β-diketonato)diorganotin(IV) derivatives containing bulky 4-acyl-5-pyrazolonato ligands : Influence of the steric hindrance of the acyl moiety on the solid state structures of tin complexes and their behaviour in solution. Inorganica Chimica Acta, Vol.367 (No.1). pp. 73-84. doi:10.1016/j.ica.2010.12.008
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Official URL: http://dx.doi.org/10.1016/j.ica.2010.12.008
Abstract
New (Q)2SnR2 derivatives (HQ in general; in detail: HQCHPh2 = 4-diphenylacetyl-3-methyl-1-phenyl-5-pyrazolone; HQBn = 3-methyl-1-phenyl-4-phenylacetyl-5-pyrazolone; HQnaph = 3-methyl-4-naphthoyl-1-phenyl-5-pyrazolone; R = CH3, C2H5, C6H11, n- and t-C4H9, C6H5,) have been synthesised and characterised by analytical and spectral techniques. Variable temperature NMR studies of (QCHPh2)2SnR2 derivatives (R = CH3 and C2H5) in chlorohydrocarbon solvents indicate a fluxional behaviour, with rapid interconversion between six- and five-coordinate species, the latter containing a bidentate acylpyrazolonate and a monodentate one. The X-ray crystal structures of the diorganotin(IV) derivatives (QCHPh2)2SnMe2, (QCHPh2)2SnEt2, (QBn)2SnMe2 and , inclusive of a representative of each Qx family, show the metal centres in a skewed trans octahedral configuration. The 4-acyl moiety of the β-diketonate donor exerts a steric effect which is correlated to structural behaviour in the solid and solution state. A solid state 119Sn CPMAS NMR study of the (QBn)2SnR2 (R = CH3, C2H5, t-C4H9 and C6H5) complexes shows a marked deshielding effect and upfield movement of the 119Sn isotropic chemical shift (δiso) through this series. The 119Sn chemical shift spans (Ω) are the largest reported for directly oxo-coordinated Sn(IV) systems, although the markedly reduced Ω value for the (QBn)2SnPh2 complex may be indicative of a cis octahedral coordination, in contrast to the trans octahedral coordination characterising the other complexes of this suite.
| Item Type: | Journal Article | ||||
|---|---|---|---|---|---|
| Subjects: | Q Science > QC Physics Q Science > QD Chemistry |
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| Divisions: | Faculty of Science > Physics | ||||
| Library of Congress Subject Headings (LCSH): | Crystallography, Nuclear magnetic resonance, Pyrazolones, Solid state physics | ||||
| Journal or Publication Title: | Inorganica Chimica Acta | ||||
| Publisher: | Elsevier BV | ||||
| ISSN: | 00201693 | ||||
| Official Date: | 28 February 2011 | ||||
| Dates: |
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| Volume: | Vol.367 | ||||
| Number: | No.1 | ||||
| Page Range: | pp. 73-84 | ||||
| DOI: | 10.1016/j.ica.2010.12.008 | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access | ||||
| Funder: | Università di Camerino, Consiglio nazionale delle ricerche (Italy) (CNR) , Vassar College , Engineering and Physical Sciences Research Council (EPSRC), University of Warwick , Advantage West Midlands (AWM) , European Regional Development Fund (ERDF) , Camille and Henry Dreyfus Foundation |
Data sourced from Thomson Reuters' Web of Knowledge
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