Atomic structure of Beta-tantalum nanocrystallites.

The structural properties of beta-phase tantalum nanocrystallites prepared by room temperature magnetron sputter deposition on amorphous carbon substrates are investigated at atomic resolution. For these purposes spherical aberration-corrected high-resolution transmission electron microscopy is applied in tandem with the numerical retrieval of the exit-plane wavefunction as obtained from a through-focus series of experimental micrographs. We demonstrate that recent improvements in the resolving power of electron microscopes enable the imaging of the atomic structure of beta-tantalum with column spacings of solely 0.127 nm with directly interpretable contrast features. For the first time ever, we substantiate the existence of grain boundaries of 30 degrees tilt type in beta-Ta whose formation may be well explained by atomic agglomeration processes taking place during sputter deposition.     

Prediction of the glass transition temperature for compatible polymer blends of varying compositions

Compatible polymer blends have been found to have widespread commercial applications. The simplest criterion for judging polymer—polymer miscibility in the solid state is the glass transition temperature (T_g), which can vary widely according to blend composition for a compatible system.Recently, an equation which predicts the T_g of intimate mixtures of compatible polymers has been derived, based on classical thermodynamics. Only a knowledge of the T_g and heat capacity increment (ΔC_p) of each pure component is required to predict the T_g at any composition.In this paper, the validity of this entropy-based relationship is investigated for a variety of commercial compatible polymer blends, including some based on poly(vinyl chloride), polystyrene, and poly(2,6-dimethyl-,4-phenylene oxide). The T_g and ΔC_p of each pure component are measured with a Perkin-Elmer DSC-2 differential scanning calorimeter, are predicted glass transition temperatures are compared with those observed experimentally.     

BINAS - synthesis and use of a new ligand for propylene hydroformylation

BINAS is a new, very efficient ligand for propylene hydroformylation. BINAS is made by the sulfonation of NAPHOS. Different synthetic routes to NAPHOS are discussed. A new two step synthesis starting from 2,2′-bis(bromomethyl)-1,1′-binaphthyl is described.     

Über Blei-haltige Heterocyclen. II. Diphenyl-substituierte Thiaplumbocane,intra- und intermolekulare Koordinationserweiterung an tetraedrisch koordinierten PbIV -Atomen

On Heterocvclic Systems Containing Lead. II. Diphenyl Substituted Thiaplumbocanes, Examples for Expanding Coordination Tetrahedra around Pb^IV 5, 5-Diphenyl-1, 4, 6, 5-oxadithiaplumbocane (PbO8Ph2) and 2, 2-diphenyl-1, 3, 6, 2-trithiaplumbocane (PbS8Ph2) have been synthesized from diphenyl lead diacetate and the respective disodium dithiolates. The mass spectra point to rearrangements induced by reduction of Pb^IV to Pb^II in addition to fragments containing Pb^IV. ¹³C and ²⁰⁷Pb NMR spectra exhibit a weaker 1, 5-transannular interaction S …? Pb than O …? Pb. The crystal structures of two modifications of PbO8Ph2 (orthorhombic and triclinic) have been determined at ? 160°C and refined to R = 0.027 and 0.071. The two modifications contain four 8-membered rings crystallographical independent, three times chair-chair, once boat-chair conformation. Eight independent Pb^IV? S single bond distances range from 248.2(3) to 251.9(6) pm. The tetrahedral C₂PbS₂ configuration is expanded by one 1,5-transannular O …? Pb interaction (285,5(5) to 308(1) pm, monocapped) and further in the triclinic case by one intermolecular S …? Pb interaction (411(1) and 375(1) pm, bicapped). The crystal structure of the orthorhombic modification contains layers (8-membered ring) (phenyl)₂ analogous to the structure of CdI₂. In the triclinic case there are dimers arranged in analogy to the cubic closest packing.     

Advances in Organophosphorus Chemistry Based on Dichloro(methyl)phosphane

Besides phosphorus trichloride and phosphane, dichloro(methyl)phosphane is gaining importance as a starting material for the synthesis of organophosphorus compounds. It provides ready access to phosphonic, phosphinic and phosphonous acid derivatives, as well as their secondary products. The synthetic and application potential of organophosphorus compounds—based on industrially produced dichloro(methyl)phosphane—is illustrated by means of numerous examples.