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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
Title | Solid-state carbon-13 nuclear magnetic resonance investigations of bismuth citrate complexes and crystal structure of Na2[Bi2(cit)2]·7H2O |
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Authors | |
Issue Date | 1996 |
Citation | Journal Of The Chemical Society - Dalton Transactions, 1996 n. 12, p. 2417-2422 How to Cite? |
Abstract | The 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 Identifier | http://hdl.handle.net/10722/168050 |
ISSN | |
ISI Accession Number ID | |
References |
DC Field | Value | Language |
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dc.contributor.author | Barrie, PJ | en_US |
dc.contributor.author | Djuran, MI | en_US |
dc.contributor.author | Mazid, MA | en_US |
dc.contributor.author | Mcpartlin, M | en_US |
dc.contributor.author | Sadler, PJ | en_US |
dc.contributor.author | Scowen, IJ | en_US |
dc.contributor.author | Sun, H | en_US |
dc.date.accessioned | 2012-10-08T03:14:33Z | - |
dc.date.available | 2012-10-08T03:14:33Z | - |
dc.date.issued | 1996 | en_US |
dc.identifier.citation | Journal Of The Chemical Society - Dalton Transactions, 1996 n. 12, p. 2417-2422 | en_US |
dc.identifier.issn | 0300-9246 | en_US |
dc.identifier.uri | http://hdl.handle.net/10722/168050 | - |
dc.description.abstract | The 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.language | eng | en_US |
dc.relation.ispartof | Journal of the Chemical Society - Dalton Transactions | en_US |
dc.title | Solid-state carbon-13 nuclear magnetic resonance investigations of bismuth citrate complexes and crystal structure of Na2[Bi2(cit)2]·7H2O | en_US |
dc.type | Article | en_US |
dc.identifier.email | Sun, H:hsun@hkucc.hku.hk | en_US |
dc.identifier.authority | Sun, H=rp00777 | en_US |
dc.description.nature | link_to_subscribed_fulltext | en_US |
dc.identifier.doi | 10.1039/DT9960002417 | - |
dc.identifier.scopus | eid_2-s2.0-33749094187 | en_US |
dc.relation.references | http://www.scopus.com/mlt/select.url?eid=2-s2.0-33749094187&selection=ref&src=s&origin=recordpage | en_US |
dc.identifier.issue | 12 | en_US |
dc.identifier.spage | 2417 | en_US |
dc.identifier.epage | 2422 | en_US |
dc.identifier.isi | WOS:A1996UU18700004 | - |
dc.identifier.scopusauthorid | Barrie, PJ=7004089987 | en_US |
dc.identifier.scopusauthorid | Djuran, MI=6701908704 | en_US |
dc.identifier.scopusauthorid | Mazid, MA=7003655997 | en_US |
dc.identifier.scopusauthorid | McPartlin, M=7006299312 | en_US |
dc.identifier.scopusauthorid | Sadler, PJ=7103024488 | en_US |
dc.identifier.scopusauthorid | Scowen, IJ=6701763189 | en_US |
dc.identifier.scopusauthorid | Sun, H=7404827446 | en_US |
dc.identifier.issnl | 0300-9246 | - |