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231223s2009 xx |||||o 00| ||eng c |
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|a 10.1002/mrc.2446
|2 doi
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|a pubmed25n0629.xml
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|a (NLM)19444858
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|a DE-627
|b ger
|c DE-627
|e rakwb
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|a eng
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1 |
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|a Chandrashekhar, N
|e verfasserin
|4 aut
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|a Synthesis of rhodium(III) complexes with tris/tetrakis-benzimidazoles and benzothiazoles--quick identification of cyclometallation by nuclear magnetic resonance spectroscopy
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|c 2009
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|a Text
|b txt
|2 rdacontent
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|a ƒaComputermedien
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|2 rdamedia
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|a ƒa Online-Ressource
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|a Date Completed 16.09.2009
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|a Date Revised 08.07.2009
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|a published: Print
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|a Citation Status PubMed-not-MEDLINE
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|a Reactions of rhodium(III) halides with multidentate N,S-heterocycles, (LH3) 1,3,5-tris(benzimidazolyl)benzene (L1H3; 1), 1,3,5-tris(N-methylbenzimidazolyl) benzene (L2H3; 2) and 1,3,5-tris(benzothiazolyl)benzene (L3H3; 3), in the molar ratio 1:1 in methanol-chloroform produced mononuclear cyclometallated products of the composition [RhX2(LH2)(H2O)] (X = Cl, Br, I; LH2 = L1H2, L2H2, L3H2). When the metal to ligand (1-3 or 1,2,4,5-tetrakis(benzothiazolyl)benzene [L4H2; 4]) molar ratio was 2:1, the reactions yielded binuclear complexes of the compositions [Rh2Cl5(LH2)(H2O)3] (LH2 = L1H2, L2H2, L3H2) and [Rh2X4(L4)(H2O)2] (X = Cl, Br, I). Elemental analysis, IR and 1H nuclear magnetic resonance (NMR) chemical shifts supported the binuclear nature of the complexes. Cyclometallation was detected by conventional 13C NMR spectra that showed a doublet around approximately 190 ppm. Cyclometallation was also detected by gradient-enhanced heteronuclear multiple bond correlation (g-HMBC) experiment that showed cross-peaks between the cyclometallated carbon and the central benzene ring protons of 1-3. Cyclometallation was substantiated by two-dimensional 1H-1H correlated experiments (gradient-correlation spectroscopy and rotating frame Overhauser effect spectroscopy) and 1H-13C single bond correlated two-dimensional NMR experiments (gradient-enhanced heteronuclear single quantum coherence). The 1H-15N g-HMBC experiment suggested the coordination of the heterocycles to the metal ion via tertiary nitrogen
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|a Journal Article
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|a Gayathri, V
|e verfasserin
|4 aut
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|a Nanje Gowda, N M
|e verfasserin
|4 aut
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|i Enthalten in
|t Magnetic resonance in chemistry : MRC
|d 1985
|g 47(2009), 8 vom: 15. Aug., Seite 666-73
|w (DE-627)NLM098179667
|x 1097-458X
|7 nnns
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| 773 |
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|g volume:47
|g year:2009
|g number:8
|g day:15
|g month:08
|g pages:666-73
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|u http://dx.doi.org/10.1002/mrc.2446
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