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Synthesis and structure of new oligomethylene-bridged double ladders. How far can the layers be separated?

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journal contribution
posted on 2004-01-01, 00:00 authored by J Beckmann, Dainis Dakternieks, Andrew DuthieAndrew Duthie, Fong Sheen Kuan, K Jurkschat, M Schurmann, E Tiekink
The synthesis of the α,ω-bis[dichloro(trimethylsilylmethyl)stannyl]alkanes, (Me3SiCH2)C12Sn(CH2)nSnCl2(CH2SiMe3) (13, n=5; 14, n=6; 15, n=7; 16, n=8; 17, n=10; 18, n=12) and the corresponding oligomethylene-bridged diorganotin oxides [(Me3SiCH2)(O)Sn(CH2)nSn(O)(CH2SiMe3)]m (19, n=5; 20, n=6; 21, n=7; 22, n=8; 23, n=10; 24; n=12) is reported. The reaction of the diorganodichlorostannanes 13–18 with the corresponding diorganotin oxides 19–24 provided the spacer-bridged tetraorganodistannoxanes {[(Me3SiCH2)ClSn(CH2)nSnCl(CH2SiMe3)]O}4 (25, n=5; 26, n=6; 27, n=7; 28, n=8; 29, n=10; 30, n=12). Compounds 13–30 have been identified by elemental analyses and multinuclear NMR spectroscopy. Compounds 25, 27, 29 and 30 have also been characterised by single crystal X-ray diffraction analysis and electrospray mass spectrometry. For the latter the essential double ladder motif is maintained for all n in the solid state, but subtle changes in alignment of the ladder planes occur. Separation between the two layers of the double ladder ranges from approx. 8.7  Å (for 25, n=5) to approx. 15 Å (for 30, n=12). In solution there is some dissociation of the double ladders into the corresponding dimers. The degree of dissociation is favoured by increasing oligomethylene chain length n.


History

Journal

New journal of chemistry

Volume

2004

Pagination

1268 - 1276

Location

Cambridge, England

Open access

  • Yes

ISSN

1144-0546

eISSN

1369-9261

Language

eng

Notes

First published on the web 16th September 2004

Publication classification

C1 Refereed article in a scholarly journal; C Journal article

Copyright notice

2004, The Royal Society of Chemistry