Synthesis and crystal structure of [{nBuMg(μ-TMP)}2] and of a homometallic inverse crown in tetranuclear [{nBuMg2[μ-N(H)Dipp] 2(μ3-OnBu)}2]

Angewandte Chemie - International Edition

Volumn 43, Issue 13, 2004, Pages 1709-1712

  Hevia, Eva ^a   Kennedy, Alan R ^a   Mulvey, Robert E ^a   Weatherstone, Susan ^a  

^a UNIVERSITY OF STRATHCLYDE   (United Kingdom)

Author keywords

Alkoxides; Amides; Crown compounds; Inverse crown compounds; Magnesium

Indexed keywords

ALKALI METALS; MAGNESIUM PRINTING PLATES; POSITIVE IONS; SYNTHESIS (CHEMICAL);

AMIDES; HETEROMETALLIC COMPOUNDS;

CRYSTAL STRUCTURE;

ALKALI METAL; CATION; HYDROGEN; MAGNESIUM DERIVATIVE; METAL DERIVATIVE; METAL ION; NITROGEN DERIVATIVE;

ARTICLE; CARBON NUCLEAR MAGNETIC RESONANCE; CHEMICAL COMPOSITION; CHEMICAL STRUCTURE; CRYSTAL STRUCTURE; PROTON NUCLEAR MAGNETIC RESONANCE; SYNTHESIS;

CRYSTALLIZATION; CRYSTALLOGRAPHY, X-RAY; MAGNESIUM; MODELS, MOLECULAR; MOLECULAR STRUCTURE; ORGANOMETALLIC COMPOUNDS;

EID: 4544334141     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/anie.200353286     Document Type: Article

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17. -3. H atoms of the four methyl groups in close contact with the Mg center were refined isotropically but all other H atoms were placed in calculated positions and in riding modes.
18. In a typical experiment the total alkalinity was found to be 10% percent higher than the alkalinity attributed exclusively to the BuMgCl. We assume that this is due to the presence of alkoxide in the solution, as was later confirmed by the NMR data, see reference [15]. For details of the double titration method see: M. Schlosser, Organometallics in Synthesis, Wiley, Chichester, 2002, p. 295.
19. 2 group is found.
20. -3. The quality of the structure solution is adversely affected by disorder in one butyl group and one amide ligand. Each was modeled as disordered over two sites. The NH atoms were refined isotropically but all other H atoms were placed in calculated positions and in riding modes. CCDC-223758 (1) and CCDC-223759 (2) contain the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB21EZ, UK; fax: (+ 44)1223-336-033; or deposit@ccdc.cam.ac.uk).
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