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Article: Solid-state carbon-13 nuclear magnetic resonance investigations of bismuth citrate complexes and crystal structure of Na2[Bi2(cit)2]·7H2O

TitleSolid-state carbon-13 nuclear magnetic resonance investigations of bismuth citrate complexes and crystal structure of Na2[Bi2(cit)2]·7H2O
Authors
Issue Date1996
Citation
Journal Of The Chemical Society - Dalton Transactions, 1996 n. 12, p. 2417-2422 How to Cite?
AbstractThe complex Na2[Bi2(cit)2]·7H2O (H4cit = 3-carboxy-3-hydroxypentane-1,5-dioic acid) crystallized during reactions of the antiulcer drug ranitidine bismuth citrate with the tripeptide glutathione (γ-L-Glu-L-Cys-Gly) at low pH. X-Ray analysis showed one [Bi(cit)]- fragment per asymmetric unit with Bi3+ chelated to a terminal carboxylate group; citrate also binds, in tridentate mode, to the bismuth of an equivalent [Bi(cit)]- unit (related to the first by a C2 axis) via one oxygen donor from each of the remaining two carboxylate groups and the alkoxy group. Both ends of the resultant dimeric anion {Bi(μ-cit)2Bi}2- bind to adjacent dimers, related by n-glide plane symmetry, via double carboxylate bridges, to form a continuous polymeric anionic chain [{Bi(μ-cit)2Bi}n]2n- running throughout the crystal. In this way each bismuth atom achieves six-co-ordination [Bi-O 2.210(10)-2.505(10) Å] with a nido-pentagonal-bipyramidal geometry, the vacant axial site providing evidence for a stereochemically active lone pair and the second axial site being occupied by the alkoxy donor. The parallel polyanionic chains are linked by anion-cation interactions [Na ⋯ O (cit) 2.37-2.50 Å] and by bonds of largely ionic character (Bi ⋯ O 3.003-3.095 Å) to give the overall three-dimensional solid-state structure which incorporates seven water molecules per dianionic subunit. The solid-state cross-polarization magic angle spinning 13C NMR spectrum of this complex is assigned with the aid of dipolar-dephasing and inversion-recovery cross-polarization experiments, and compared to those of ranitidine bismuth citrate and bismuth citrate Bi(Hcit). The IR and solid-state 13C NMR data suggested that the alkoxy group is protonated in Bi(Hcit) but deprotonated in ranitidine bismuth citrate, and that the latter contains similar dimeric units to Na2[Bi2(cit)2]·7H2O. The general modes of aggregration of dimeric [{Bi(μ-cit)2Bi}n]2n- units and the relevance to antiulcer activity are discussed.
Persistent Identifierhttp://hdl.handle.net/10722/168050
ISSN
1999 Impact Factor: 2.31
ISI Accession Number ID
References

 

DC FieldValueLanguage
dc.contributor.authorBarrie, PJen_US
dc.contributor.authorDjuran, MIen_US
dc.contributor.authorMazid, MAen_US
dc.contributor.authorMcpartlin, Men_US
dc.contributor.authorSadler, PJen_US
dc.contributor.authorScowen, IJen_US
dc.contributor.authorSun, Hen_US
dc.date.accessioned2012-10-08T03:14:33Z-
dc.date.available2012-10-08T03:14:33Z-
dc.date.issued1996en_US
dc.identifier.citationJournal Of The Chemical Society - Dalton Transactions, 1996 n. 12, p. 2417-2422en_US
dc.identifier.issn0300-9246en_US
dc.identifier.urihttp://hdl.handle.net/10722/168050-
dc.description.abstractThe complex Na2[Bi2(cit)2]·7H2O (H4cit = 3-carboxy-3-hydroxypentane-1,5-dioic acid) crystallized during reactions of the antiulcer drug ranitidine bismuth citrate with the tripeptide glutathione (γ-L-Glu-L-Cys-Gly) at low pH. X-Ray analysis showed one [Bi(cit)]- fragment per asymmetric unit with Bi3+ chelated to a terminal carboxylate group; citrate also binds, in tridentate mode, to the bismuth of an equivalent [Bi(cit)]- unit (related to the first by a C2 axis) via one oxygen donor from each of the remaining two carboxylate groups and the alkoxy group. Both ends of the resultant dimeric anion {Bi(μ-cit)2Bi}2- bind to adjacent dimers, related by n-glide plane symmetry, via double carboxylate bridges, to form a continuous polymeric anionic chain [{Bi(μ-cit)2Bi}n]2n- running throughout the crystal. In this way each bismuth atom achieves six-co-ordination [Bi-O 2.210(10)-2.505(10) Å] with a nido-pentagonal-bipyramidal geometry, the vacant axial site providing evidence for a stereochemically active lone pair and the second axial site being occupied by the alkoxy donor. The parallel polyanionic chains are linked by anion-cation interactions [Na ⋯ O (cit) 2.37-2.50 Å] and by bonds of largely ionic character (Bi ⋯ O 3.003-3.095 Å) to give the overall three-dimensional solid-state structure which incorporates seven water molecules per dianionic subunit. The solid-state cross-polarization magic angle spinning 13C NMR spectrum of this complex is assigned with the aid of dipolar-dephasing and inversion-recovery cross-polarization experiments, and compared to those of ranitidine bismuth citrate and bismuth citrate Bi(Hcit). The IR and solid-state 13C NMR data suggested that the alkoxy group is protonated in Bi(Hcit) but deprotonated in ranitidine bismuth citrate, and that the latter contains similar dimeric units to Na2[Bi2(cit)2]·7H2O. The general modes of aggregration of dimeric [{Bi(μ-cit)2Bi}n]2n- units and the relevance to antiulcer activity are discussed.en_US
dc.languageengen_US
dc.relation.ispartofJournal of the Chemical Society - Dalton Transactionsen_US
dc.titleSolid-state carbon-13 nuclear magnetic resonance investigations of bismuth citrate complexes and crystal structure of Na2[Bi2(cit)2]·7H2Oen_US
dc.typeArticleen_US
dc.identifier.emailSun, H:hsun@hkucc.hku.hken_US
dc.identifier.authoritySun, H=rp00777en_US
dc.description.naturelink_to_subscribed_fulltexten_US
dc.identifier.doi10.1039/DT9960002417-
dc.identifier.scopuseid_2-s2.0-33749094187en_US
dc.relation.referenceshttp://www.scopus.com/mlt/select.url?eid=2-s2.0-33749094187&selection=ref&src=s&origin=recordpageen_US
dc.identifier.issue12en_US
dc.identifier.spage2417en_US
dc.identifier.epage2422en_US
dc.identifier.isiWOS:A1996UU18700004-
dc.identifier.scopusauthoridBarrie, PJ=7004089987en_US
dc.identifier.scopusauthoridDjuran, MI=6701908704en_US
dc.identifier.scopusauthoridMazid, MA=7003655997en_US
dc.identifier.scopusauthoridMcPartlin, M=7006299312en_US
dc.identifier.scopusauthoridSadler, PJ=7103024488en_US
dc.identifier.scopusauthoridScowen, IJ=6701763189en_US
dc.identifier.scopusauthoridSun, H=7404827446en_US

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