Organoboron compounds. Communication 136. Boron-germanium compounds

Summary Triethyl- and triphenyl-germanes add to dimethyl 2-propene-1-boronate with formation of dimethyl 3-(triethylgermyl)- and 3-(triphenylgermyl)-1-propaneboronates respectively.The NMR spectrum was measured by V. F. Bystrov, whom the authors thank. The authors also thank V. F. Mironov for the provision of a sample of 3-(triethylgermyl)-1-propanol.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 1, pp. 68–72, January, 1965     

Polymerization studies on allylic compounds. IV. Methallylic compounds

The free-radical polymerization of a series of 2-methyl-3-substituted propenes was investigated. These compounds were found to homopolymerize with difficulty to give low molecular weight polymers. Their effect upon the polymerization of methyl methacrylate and styrene was investigated by rate and viscosity measurements. Copolymerizations occurred with a retarding action attributed to pronounced chain transfer reactions.     

Ferrocene compounds. XXXIX.

In the title compound, [Fe(C₅H₅)(C₁₄H₁₃O)], the plane of the heterocyclic ring is almost perpendicular to the plane of the substituted cyclo­penta­dienyl ring, and the heterocyclic ring adopts a half‐chair conformation. The conformation of the nearly parallel cyclo­penta­dienyl (Cp) rings [the dihedral angle between their planes is 2.7 (1)°] is almost halfway between eclipsed and staggered, and the rings are mutually twisted by about 19.4 (2)° (mean value). The mean lengths of the C—C bonds in the substituted and unsubstituted cyclo­penta­dienyl ring are 1.420 (2) and 1.406 (3) Å, respectively, and the Fe—C distances range from 2.029 (2) to 2.051 (2) Å. The phenyl and unsubstituted cyclo­penta­dienyl rings are involved in C—H⃛π interactions, with intermolecular H⃛centroid distances of 2.85 and 3.14 Å for C—H⃛π(Ph), and 2.88 Å for C—H⃛π(Cp). In two of these interactions, the C—H bond points towards one of the ring bonds rather than towards the ring centroid. In the crystal structure, the C—H⃛π interactions connect the mol­ecules into a three‐dimensional framework.     

Cyclometallated compounds. XV.

The title complex, tetra‐μ‐acetato‐O:O′‐bis{[μ‐1,4‐bis(2‐­pyridyl­oxy)­phenyl­ene‐N,C²:N′,C⁶]dipalladium(II)} bis­(tri­chloro­methane) dihydrate, [Pd₄(C₁₆H₁₀N₂O₂)₂(C₂H₃O₂)₄]·2CHCl₃·2H₂O, the product of the reaction of 1,4‐bis(2‐pyridyl­oxy)­benzene with palladium acetate, is shown to be a tetranuclear, rather than a polymeric, species. It crystallizes about a centre of inversion and has two doubly cyclo­palladated ligands bridged by four acetate groups. The cyclo­palladated ligand is far from planar in the complex and has the central benzene rings π‐stacked. The chelate rings exist in shallow boat conformations.     

GPC analysis of model compounds. I. Phenyl- and benzo-substituted aromatic compounds

A series of 36 compounds of known structure was used in a study to elucidate the mechanism of separation of gel-permeation chromatography (GPC). The various molecular dimensions were defined and measured for these compounds. The elution volume for these compounds was determined by GPC under specified and controlled conditions. The relationships between elution volume and molecular dimension were investigated using computer-based statistical analysis for the entire set of compounds and manual simultaneous equations for smaller sets of compounds. It was found that, as increasingly more molecular dimensions are considered, (1) the importance of the maximum molecular dimension A_p′ (the only dimension considered by many investigators) significantly decreases and (2) a significantly better prediction of the elution volume of these compounds could be made.     

Nitrogen-containing organosiligon compounds.

A. Number of new 4-[Y-(trialkylsilyl)propylamino]quinolines and their hydrochlorides were synthesized by heating 4-chloroquinolines with trialkyl(3-aminopropyl)-silanes in phenol or diglyme. The antimicrobial activity of the products was determined.