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1.
Acta Crystallogr C ; 62(Pt 10): m458-60, 2006 Oct.
Article in English | MEDLINE | ID: mdl-17008728

ABSTRACT

The title compound, (C16H20N)2[Fe2Br6O], crystallizes with one dibenzyldimethylammonium cation and one half of a mu-oxo-bis[tribromoferrate(III)] anion in the asymmetric unit. The bridging oxo group is situated on an inversion centre, resulting in a linear conformation for the Fe-O-Fe unit. The iron(III) cations have tetrahedral geometry, with bond angles in the range 106.8 (1)-112.2 (1) degrees . The ion pairs are held together by Coulombic forces and C-H...Br hydrogen bonds. Each Br- anion forms one hydrogen bond. No C-H...O hydrogen bonds are found between the O atom in the Fe-O-Fe unit and surrounding counter-cations, consistent with the linear configuration of the Fe-O-Fe unit.


Subject(s)
Iron/chemistry , Oxygen/chemistry , Quaternary Ammonium Compounds/chemistry , Crystallography, X-Ray , Hydrogen Bonding , Models, Molecular , Molecular Structure
2.
Chemistry ; 12(16): 4289-96, 2006 May 24.
Article in English | MEDLINE | ID: mdl-16568487

ABSTRACT

The assembly of C-methyl resorcinarene into a tubular supramolecular solid-state structure, its thermal stability, and its hosting properties are reported. Careful control of the crystallisation conditions of C-methyl resorcinarene and 1,4-dimethyl-1,4-diazoniabicyclo[2.2.2]octane (1,4-dimethyl DABCO) dibromide leads to a formation of two crystallographically different, but structurally very similar, solid-state nanotube structures. These structures undergo a remarkable variety of supramolecular interactions, which lead to the formation of 0.5 nm diameter nonpolar tubes through the crystal lattice. The formation of these tubes is templated by suitably sized small alcohols, namely, n-propanol, 2-propanol, or n-butanol. The self-assembly involves close pi...pi interactions between the adjacent resorcinarenes, and C--H...pi and cation...pi interactions between the resorcinarenes and the guest 1,4-dimethyl DABCO dications. The crystals of these supramolecular tube structures are thermally very stable and the included solvent alcohol can be removed from the tubes without breaking the single-crystalline structure of the assembly. After removal of the solvent molecules the tubes can be filled with other small, less polar solvent molecules such as dichloromethane.


Subject(s)
Hot Temperature , Nanotubes/chemistry , Phenylalanine/analogs & derivatives , Calixarenes , Crystallization , Molecular Conformation , Phenylalanine/chemistry , Piperazines/chemistry , Solvents/chemistry
3.
Anal Chim Acta ; 580(1): 91-8, 2006 Oct 27.
Article in English | MEDLINE | ID: mdl-17723760

ABSTRACT

This study presents the use of quaternary ammonium bromides as additives in N-methylformamide (NMF) for the separation and quantification of chelating agents as copper complexes by capillary zone electrophoresis (CZE). The new quaternary ammonium bromides were synthesized in our laboratory and used for the first time for CZE applications performed in NMF media. The methods were developed and optimized for determination of six chelating agents (trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid (HEDTA), nitrilotriacetic acid (NTA) and triethylenetetraaminehexaacetic acid (TTHA)) as copper complexes. Among the tested electrolyte additives in NMF media (pH(app) 10.2) dimethyldioctylammonium bromide (DMDOAB), dimethyldinonylammonium bromide (DMDNAB) and dimethyldidecylammonium bromide (DMDDAB), at a concentration of 20 mmol L(-1) improved the separation of the copper complexes. The optimized methods require only 12 min for one analysis, and the detection limits for copper complexes of DMDNAB, the best-performing additive, were < or =24 micromol L(-1). Relative standard deviations (R.S.D.) for migration times were < or =2.5, < or =2.1, < or =3.1% and for peak areas, < or =3.1, < or =3.0, < or =3.2% for DMDOAB, DMDNAB and DMDDAB used as additives, respectively. All three methods were successfully applied to the analysis of natural and wastewater samples. No matrix effects from these samples were observed. The interaction between quaternary ammonium bromides and copper complexes is discussed.

4.
J Chromatogr A ; 1095(1-2): 164-71, 2005 Nov 18.
Article in English | MEDLINE | ID: mdl-16275297

ABSTRACT

Two new methods of capillary zone electrophoresis based on aqueous phosphate running buffers with UV spectrophotometric detection were developed and optimized for the determination of eight carboxylates as copper complexes. Metalcomplexes are negatively charged, so measurements were made as anion analyses with flow reversal in the capillary. Two flow modifiers were used: a common tetradecyltrimethylammonium bromide (TTAB) and a new ionic liquid dimethyldinonylammonium bromide (DMDNAB). The methods were compared to each other. Better separation was achieved with DMDNAB as the flow modifier. Method development was done using a fused silica capillary (61 cm x 50 microm i.d.). Optimization was done using 95 mmol L(-1) phosphate buffer with TTAB or DMDNAB in the concentration 0.5 mmol L(-1) at pH 7.1. A -20 kV voltage and direct UV detection at 254 nm was used in measurements. In both CE methods all the peaks in the electropherograms were properly separated, the calibration plots gave good correlation coefficients and all eight carboxylates were detected in less than 7.5 min. The two methods were tested with natural water samples and a paper mill sample, and proved to be feasible.


Subject(s)
Carboxylic Acids/analysis , Electrophoresis, Capillary/methods , Quaternary Ammonium Compounds/chemistry , Electrophoresis, Capillary/instrumentation , Spectrophotometry, Ultraviolet , Trimethyl Ammonium Compounds , Water Pollutants, Chemical/analysis
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