Geometries of type Cn and F4 with flag-transitive automorphism groups

Let be a finite thick geometry of type C_n (n 4) or F₄. We prove that is a building iff Aut() is flag-transitive.     

A validated spectrofluorometric method for the determination of celecoxib in capsules

A rapid, selective, sensitive and simple fluorescence method was developed for the direct determination of celecoxib in capsules. The capsules were emptied, pulverized and dissolved in either ethanol or acetonitrile, sonicated and filtered. Direct fluorescence emission was measured at 355±5 nm (exciting at 272 nm). The method was fully validated and the recoveries were excellent, even in presence of excipients.     

DAC-FECS Affairs

DAC-FECS Affairs

The Division of Analytical Chemistry     

Crystal and molecular structure of nitrosyl(1,10-phenanthroline)-bis(triphenylphosphine)iridium(I) Dihexafluorophosphate, [Ir(NO)(phen)(PPh3)2][PF6]2

Summary The structure of [Ir(NO)(phen)(PPh₃)₂][PF₆]₂ has been determined from x-ray diffractometer data. The compound crystallizes in space groupPnam with four molecules in a unit cell witha = 19.924(12),b = 14.793(9) andc = 16.348(9) A. Full-matrix least-squares refinement has led to a final R value of 0.061 for the 4796 observed reflections. The structure consists of well-separated ions, and the geometry around the metal is trigonal bipyramidal with nitrosyl and bidentate 1,10-phenanthroline (in spite of the very narrow bite angle of 75.8°) ligands occupying the equatorial positions and the triphenylphosphine ligands the axial positions. The cation has an imposed crystallographicm symmetry. Important bond lengths are as follows: Ir-P, 2.391(3): Ir-N (nitrosyl) 1.700(12): Ir-N (1,10-phenanthroline) 2.103(12) and 2.142(11): N-O, 1.201(18)A. The nitrosyl ligand is linear [Ir-N-O = 179.9(9)°] so that this complex can be formulated as an NO⁺ complex of iridium(I).     

Indirect automatic atomic absorption determination of sulphate based on its precipitation with barium

A continuous precipitation flame atomization atomic absorption spectrometric method for the indirect determination of sulphate is proposed. By using a reversed flow-injection configuration for precipitation as barium sulphate, this anion was determined in the range 10–150 g/ml, with a relative standard deviation of 2.6%. The sensitivity was increased by a factor of seven by using a nitrous oxide-acetylene flame to measure barium.     

A comparative study of several HPLC methods for determining free amino acid profiles in honey

A study of the viability of three derivatizing reagents for obtaining amino acid profiles in honey through high performance liquid chromatography (HPLC) is presented. A method using diode array detection based on a reaction with diethyl ethoxymethylene malonate (DEMM) and two other methods using fluorescence detection based on derivatization with fluorenylmethyl chloroformate (FMOC-Cl) and 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) have been developed. The three methods yield detection limits close to the ppb level, but vary in relation to other analytical characteristics. The use of methyl chloroformate derivatives allows the profile to be obtained with the greatest sensitivity within a short time frame. On applying such methods to honey samples of diverse botanical origin, we observe that the proline values obtained are always lower than those found using the official spectrophotometric method, thereby underlining the advisability of using HPLC methods to reduce uncertainty in these results.     

From cyclopentadiene to isoxazoline-carbocyclic nucleosides: a rapid access to biological molecules through nitrosocarbonyl chemistry

A rapid access to carbocyclic nucleosides containing a fused isoxazoline ring is proposed starting from cyclopentadiene. The route involves an hetero Diels-Alder cycloaddition reaction of nitrosocarbonylbenzene followed by a 1,3-dipolar cycloaddition of nitrile oxides, cleavage of the N-O tether and elaboration of the heterocyclic aminols into nucleosides via linear construction of purine and pyrimidine heterocycles.     

Reactions of organomercury fulminates with acetylene derivatives

Organomercury fulminates react with acetylene derivatives to give unstable 3-(organomercurio)isoxazoles, which isomerize to 2-cyanoenolates. These are hydrolyzed with hydrochloric acid to the corresponding enols and are cleaved by water at the double bond. With monosubstituted acetylenes, substitution at the free position by the organomercury residue is predominant.