Über Osmiumbromide

On Osmiumbromides OsBr₄ was obtained by reaction of OsCl₄ with bromine in a closed system at 330°C and 120 bar Br₂ pressure. The compound crystallizes orthorhombic (a = 633.99(18) pm; b = 1 210.92(16) pm; c = 1 461.5(10) pm; Z = 8; space group Pbca) in a TcCl₄ type structure. OsBr₆ octahedra are connected by two common edges to \documentclass{article}\pagestyle{empty}\begin{document}${}_\infty ^1 \left[ {{\rm OsBr}_{{{\rm 2} \mathord{\left/ {\vphantom {{\rm 2} 1}} \right. \kern-\nulldelimiterspace} 1}} {\rm Br}_{{{\rm 4} \mathord{\left/ {\vphantom {{\rm 4} 2}} \right. \kern-\nulldelimiterspace} 2}} } \right]$\end{document} chains with a cis arrangement of the two non-bridging Br atoms. Mixed crystals OsBr_xCl_4?x(0 < x < 2.3) with CsCl₄ type structure are formed by reactions at lower Br₂ pressure up to 12 bar. They are built up from chains consisting of edge-sharing octahedra. The terminal atoms have a trans arrangement. Attempts to synthesize single crystals of OsBr₃ by decomposition of OsBr₄ resulted in formation of three different phases OsBr_x (3 < x < 4).     

Über Chalkogenolate. 201. Untersuchungen über Selenformamide

On Chalcogenolates. 201 Studies on Selenoformamides The yellow selenoformamides H? CSe? NH₂, H? CSe? NH? CH₃, and H? CSe? N(CH₃)₂ have been prepared by reaction of the corresponding formamide with P₂Se₅. The compounds have been characterized by means of electron absorption, infrared, and nuclear magnetic resonance spectra. The decomposition of the selenoformamides in ethanolic solution has been studied kinetically at 20.0°C. The preparation of selenoformyl dithiocarbamates was not successful.     

Über Pentafluorphenylthio-Metallkomplexe

The compounds M(CO)₅ · THF (M = Cr, Mo, W) react with sodium mercaptide, NaSR (R = C₆F₅, C₆H₅, C₂H₅), to give the mercapto-pentacarbonylmetallate anions [M(CO)₅ · · SR]^?. The preparation of some pentafluorophenylthio complexes, e. g. [(C₆H₅)₃P]₂MSC₆F₅(M = Cu, Ag, Au), [(C₆H₅)₃P]₂Hg(SC₆F₅)₂, is reported.     

Über Eisengallustinte

On Iron Gallic Ink From Iron(III) chloride and gallic acid in gels single crystals could be obtained which will be the dye-stuff of iron gallic ink. The structure consists of a hexagonal iron gallic acid 1:1 framework. The oxidation state three of the iron could be confirmed by Mössbauer and XANES spectroscopy.     

Über Lanthanorthovanadat

Crystallographic data for LaVO₄ are given. Also the infrared and Raman spectra are reported and discussed with the aid of a “factor group analysis”.     

Über 1,3,2-Benzoxathiaborole

On 1,3,2-Benzoxythioborols 2-Mercapto-4-methoxyphenol reacts with BCl₃ giving the 2-Chloro-5-methoxy-1,3,2-benzoxythioborol. This compound reacts with phenol, thiophenol, 2-mercapto-4-methoxyphenol, sec. amines, lithium butyl and lithium phenyl and the corresponding 2-substituted products are obtained. With sodium two borol rings are connected resulting a boron-boron bond. The Lewis-acid behaviour of some of this compounds is investigated.     

Über Chalkogenolate. 96 [1]. Untersuchungen über Alkalimetalltrimethylsilylcarbonate

On Chalcogenolates. 96. Studies on Trimethylsilyl Carbonates of Alkali Metals The trimethylsilyl carbonates M[O₂COSi(CH₃)₃] with M = Li, Na, K, Rb, Cs have been prepared by reaction of Co₂ with the corresponding silanolate. Infrared spectra, electron absorption spectra, ¹H-NMR spectra as well as mass spectra are communicated. In aqueous solution the equivalent conductivities of [O₂COSi(CH₃)₃]^? have been determined by means of conductivity measurements. The diffusion coefficient of the ion was calculated. The dissociation constant of trimethylsilyl carbonic acid in water at 20°C is K_a = (4,83 ± 0,5) · 10^?10. The thermodynamic data of the dissociation were calculated.     

Über chirale Methylzinkaminoalkoxide

Chiral Methylzinc Amino Alkoxides Dimethylzinc reacts with (S)‐N‐methylpyrrolidinyl‐2‐methanol, (R/S)‐1‐phenyl‐2‐(N‐methylamino)‐ethanol, and (S)‐α,α‐diphenyl‐2‐pyrrolidinyl‐2‐methanol in molar ratio 1 : 1 with formation of the corresponding methylzinc amino alkoxides 1 – 3 . As a consequence of the Zn–N‐interaction new centres of chirality containing asymmetric surrounded N‐atoms are formed. Compounds 1 – 3 were characterized by their ¹H and ¹³C nmr spectra. The crystal structures of 1 – 3 were determined by single crystal structur analysis. 1 and 2 are trimeric in solid state, 3 is forming dimeric molecules.