Über Phosphorstickstoff-Verbindungen. XXXI. Über neue viergliedrige Ringsysteme mit Stickstoff,Phosphor und Kohlenstoff im Ring

A P? N compound XI, formula see ?Inhaltsübersicht”?, has been prepared containing three interconnected four-membered rings. On chlorination of XI P₂(NCH₃)₂Cl₆ is re-formed, besides a further product being very probably compound XII with hexa-coordinated phosphorus. Interaction between the known Cl₄P(NCH₃)₂ CCl₂ and NN′-dimethyl urea yields III and another compound, VII, with phosphorous of coordination number six.     

Drying dip-coated colloidal films

We present the results from a small-angle X-ray scattering (SAXS) study of lateral drying in thin films. The films, initially 10 μm thick, are cast by dip-coating a mica sheet in an aqueous silica dispersion (particle radius 8 nm, volume fraction ?(s) = 0.14). During evaporation, a drying front sweeps across the film. An X-ray beam is focused on a selected spot of the film, and SAXS patterns are recorded at regular time intervals. As the film evaporates, SAXS spectra measure the ordering of particles, their volume fraction, the film thickness, and the water content, and a video camera images the solid regions of the film, recognized through their scattering of light. We find that the colloidal dispersion is first concentrated to ?(s) = 0.3, where the silica particles begin to jam under the effect of their repulsive interactions. Then the particles aggregate until they form a cohesive wet solid at ?(s) = 0.68 ± 0.02. Further evaporation from the wet solid leads to evacuation of water from pores of the film but leaves a residual water fraction ?(w) = 0.16. The whole drying process is completed within 3 min. An important finding is that, in any spot (away from boundaries), the number of particles is conserved throughout this drying process, leading to the formation of a homogeneous deposit. This implies that no flow of particles occurs in our films during drying, a behavior distinct to that encountered in the iconic coffee-stain drying. It is argued that this type of evolution is associated with the formation of a transition region that propagates ahead of the drying front. In this region the gradient of osmotic pressure balances the drag force exerted on the particles by capillary flow toward the liquid-solid front.     

Total synthesis of the putative structure of the lupin alkaloid plumerinine

[reaction: see text]. A stereocontrolled synthesis of quinolizidine 1, the reported structure of plumerinine, has been accomplished in 10 steps from 4-methoxypyridine. The key step is a highly facial selective intramolecular [2 + 2] photocycloaddition of a 2,3-dihydro-4-pyridone. The reported spectral data for plumerinine did not match that of our synthetic 1.     

Impurities in Magnetic Insulators Studied by Low-Temperature Nuclear Orientation

Although the effects of impurities in metallic magnets have been extensively studied there have been far fewer experiments on impurities in insulating magnets, and, in an effort to understand this problem, we have investigated the effect of impurities in various systems. In MnCl₂⋅4H₂O samples doped with 1.6, 4.0 and 6.2% Co, the ⁵⁴Mn NMRON line is significantly broadened compared to the line in the pure crystal and shows structure on the low frequency side. The nuclear spin-lattice relaxation time is also lower by an order of magnitude. ⁵⁴Mn has also been doped into FeCl₂⋅4H₂O for which a 4-sublattice structure has been proposed and some details of this structure have been obtained. This revised version was published online in September 2006 with corrections to the Cover Date.