C-13-Sn-119 correlation NMR in solution and solid-state CP/MAS NMR of bis(tributylstannyl(IV)) O-5,6-isopropylidene-L-(+)-ascorbate

Various NMR correlation techniques, H-1-C-13 HMQC, H-1-C-13 HMBC, H-1-Sn-119 HMQC with gradient enhancement, and C-13-Sn-119 HMQC, enabled a. full resonance assignment and the solution structure elucidation of bis(tributylstannyl(IV)) L-(+)-ascorbate (1) and O-5,6-isopropylidene-L-(+)-ascorbate (2)...

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Published inOrganometallics Vol. 19; no. 4; pp. 703 - 706
Main Authors Lycka, A, Micak, D, Holecek, J, Biesemans, M, Martins, JC, Willem, R
Format Journal Article
LanguageEnglish
Published WASHINGTON Amer Chemical Soc 21.02.2000
Subjects
Chemistry
Chemistry, Inorganic & Nuclear
Chemistry, Organic
Physical Sciences
Science & Technology
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Summary:Various NMR correlation techniques, H-1-C-13 HMQC, H-1-C-13 HMBC, H-1-Sn-119 HMQC with gradient enhancement, and C-13-Sn-119 HMQC, enabled a. full resonance assignment and the solution structure elucidation of bis(tributylstannyl(IV)) L-(+)-ascorbate (1) and O-5,6-isopropylidene-L-(+)-ascorbate (2) in deuteriochloroform. Double heteronuclear C-13-Sn-119 HMQC spectroscopy appeared indispensable for discriminating between (2)J(C-13-O-Sn-119) and (3)J(C-13=C-O-Sn-119) coupling pathways involving quaternary carbon atoms and provided useful information about the relative magnitudes of (2)J(C-13-Sn-119) and (3)J(C-13-Sn-119) coupling constants, as they turned out to have an uncommon coupling size sequence. While the tin atoms in compounds I and 2 are four-coordinate in solution, Sn-117 CP/MAS NMR reveals that compound 2 has one four-coordinate and one five-coordinate tin atom in the solid state.
ISSN:0276-7333
DOI:10.1021/om9907526