Embracing C(60) with multiarmed geodesic partners.

1,3,5,7,9-Pentakis(4-methoxyphenylthio)corannulene (3), 1,3,5,7,9-pentakis(2-naphthylthio)corannulene (4), and 1,3,6,8-tetrakis(4-methoxyphenylthio)corannulene (5b) have been synthesized by chlorination of corannulene with ICl in CH(2)Cl(2) at 25 degrees C and subsequent nucleophilic aromatic substitution with the appropriate sodium thiophenolate in DMEU at 25 degrees C. (1)H NMR titration studies demonstrate that these novel bowl-shaped hosts form 1:1 complexes with C(60) in toluene-d(8) solution with association constants of 454, 368, and 280 M(-1), respectively.

First synthesis of lower-rim-substituted aryl ethers of p-tert-butylcalix[4]arene.

With the use of S(N)Ar or Ullmann reactions, the synthesis of the first lower-rim aryl ether derivatives of tert-butylcalix[4]arene is reported, as are some of their conformational properties, (1)H NMR spectra, and X-ray crystal structures. The lower-rim aryl pendants reported herein provide for new scaffolds upon which a host of other new molecular architectures can be constructed, thus extending the capability of the versatile calix[4]arenes even further.

Synthesis of hexahomotrioxacalix[3]naphtalenes and a study of their alkali-metal cation binding properties.

The first syntheses of the C3-symmetrical and unsymmetrical hexahomotrioxacalix[3]naphthalenes 3 and 4, respectively, and the corresponding tert-butyl hexahomotrioxacalix[3]naphthalene 3a are reported. A convergent synthesis of the linear hexahomotrimer precursors 19 and 19a is described, but the direct synthesis of 3 and 3a can also be achieved from the monomers 20 and 20a, respectively. A limited study of the binding properties of alkali-metal cations by 3 or 3a using a picrate-CHCl3 extraction showed only weak abilities to bind with the cations examined.

Spontaneous revertants in modified S. typhimurium mutagenicity tests employing elevated numbers of the tester strain.

It has been proposed that increases in the number of bacteria applied to each plate can enhance the sensitivity of the Ames S. typhimurium mutagenicity assay. These procedures have the potential to elevate the number of spontaneous revertants (SR) by increasing the contribution of pre-existing revertants (PER) present before application of the bacteria to the limited histidine test plates. We have investigated the contribution of PER when 10(9) bacteria are applied to the plates and found that the number of PER is dependent on the handling and storage of the cultures used to inoculate the overnight broth. The average number of PER/10(9) viable bacteria after overnight growth in broths inoculated from a frozen permanent, lyophilized permanent, master plate, and an isolated colony, of TA98 were 267, 188, 57 and 13 respectively. The resultant elevation of the number of SR for a strain may result in a failure to identify a mutagenic response. It is recommended that the number of PER be monitored in any modification of the Ames test that makes use of elevated numbers of bacteria.

Luciferin-luciferase assay of adenosine triphosphate from bacteria: a comparison of dimethylsulphoxide (DMSO) and acetone with other solvents.

The extraction of adenosine triphosphate (ATP) from six strains of bacteria, chosen for differences in cell-wall composition and habitat, was performed. The solvents were two in common use, Tris-ethylenediaminetetraacetate (Tris-EDTA) and trichloroacetic acid (TCA), and two promising, though less utilized solvents, dimethylsulphoxide (DMSO) and acetone. ATP was determined by the luciferin-luciferase reaction. Of the solvents used, DMSO and acetone were the most effective considering the different kinds of bacteria tested and, of these two, DMSO was the most convenient to use. Tris-EDTA was not as effective as the other solvents tested and TCA, which was effective with most strains, gave low yields when used with cultures grown in artificial seawater broth. Internal standards were used to determine if there were substances present that could inhibit the reaction of released ATP with the luciferin-luciferase reagent. Extracts of ATP, stored at -20 degrees C, were stable for up to 3 weeks.

The mutagenicity of a Prudhoe Bay crude oil and its residues from an experimental in situ burn.

Fresh and weathered Prudhoe Bay crude oil as well as residues from its combustion were tested for mutagenicity using strain TA98 in the Ames Salmonella typhimurium/liver microsome test. Because of the toxicity of the oils involved, mutagenic effects were clearly visible only at very low concentrations. All samples were found to be mutagenic, with precipitated plume having the greatest activity followed by the burn residue, the weathered oil, and fresh crude, respectively. The most polar components of the neutral fraction of the samples displayed the greatest mutagenicity.