Trennung von Selen und Tellur mit Hilfe von Bismuthiol II

Zusammenfassung Tellur(IV) läßt sich von Selen(IV) durch Ausschütteln der Bismuthiol II-Verbindung mit Chloroform trennen. Der pH-Wert der Ausgangslösung muß zwischen pH 4,5 und 4,7 liegen, die Reagenszugabe darf erst nach der pH-Einstellung erfolgen.

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Separation of selenium and tellurium by means of Bismuthiol II

Tellurium(IV) can be separated from selenium(IV) by extracting the Bismuthiol II complex with chloroform at pH 4.5–4.7 of the aqueous solution. The addition of the organic reagent must be made after adjusting the pH.

     

Synthese und Zerfall von Azoinitiatoren,II

For further investigation of the relations between the structure and the decomposition of the azoesters of the typePhR ¹ R ²CN=CNR ² R ¹ Ph two supplement series (R ¹=CH₃, C₂H₅;R ²=substituted acetic acids) were synthesized. Especially information were obtained concerning the reasons for the low temperatures of decomposition of the azoesters of acetic acid. The azoesters of the substituted acetic acids follow a law of first order for the decomposition.     

Kolloidale und Oberflächeneigenschaften von Tonsuspensionen. II. Elektrophorese und Kationenadsorption von Montmorillonit

Ohne Zusammenfassung     

Das Austauschverhalten von Mangan(II)-ionen und von Erdalkaliionen

Ohne Zusammenfassung     

Hydratstufen und Kristallstrukturen von Strontiumchlorid und Europium(II)-chlorid

Hydrates and Crystal Structures of Strontium Chloride and Europium Dichloride The dehydrating processes of SrCl₂ · 6 H₂O and EuCl₂ · 2 H₂O and the phase transformations involved were observed using a high temperature X-ray camera. The following phases appeared with increasing temperatur in the SrCl₂? H₂O system: SrCl₂ · 6 H₂O → SrCl₂ · 2 H₂O → SrCl₂ · 1 H₂O → SrCl₂(cub), and in the EuCl₂? H₂O system: EuCl₂ · 2 H₂O → EuCl₂ · 1 H₂O → EuCl₂ · wH₂O → EuCl₂(ortho), [EuCl₂(kub)].     

Synthese und Struktur der Kronenetherkomplexe von Kaliumhexachlorodipalladat(II) und -diplatinat(II)

Synthesis and Structure of Crown Ether Complexes of Potassium Hexachlorodipalladate(II) and -diplatinate(II) K₂[MCl₄] (M ? Pd, Pt) reacts with an excess of crown ether 18-crown-6 in water to give the crown ether complexes of potassium hexachlorodipalladate(II) and -diplatinate(II) [K(18-cr-6)]₂[M₂Cl₆] (M ? Pd, 1 ; M ? Pt, 3 ), respectively, and in methylene chloride to give those of potassium tetrachloropalladate(II) and -platinate(II) [K(18-cr-6)]₂[MCl₄] ( 1 ) (M ? Pd, 2 ; M ? Pt, 4 ), respectively. 1 - 4 are characterized by microanalysis, NMR (¹H, ¹³C), and vibrational spectroscopy. The X-ray structure analyses of the isotypic complexes 1 (P2₁/c; a = 10,9678(8), b = 8,2991(7), c = 22,469(2) Å, β = 98,523(5)°; Z = 2) and 3 (P2₁/c; a = 10,934(3), b = 8.376(3), c = 22,410(5) Å, β = 98,77(3)°; Z = 2) reveal [M₂Cl₆]^2? anions of nearly D_2h symmetry and [K(18-cr-6)]⁺ cations, in which the distance of K⁺ to the mean plane of the crown ether defined by its six oxygen atoms amounts to 0,830(4) Å in 1 and 0,821(2) Å in 3 , respectively. There are tight contacts between cations and anions (d(K-Cl): 3,341(2)/3,260(2) Å ( 1 ); 3,348(4)/3,259(4) Å ( 3 )).     

Nitrosodicyanmethanid-Komplexe von Palladium(II) und Platin(II)

Crystal and Molecular Structure of 1,8-Dihydroxy-3,6-dithiaoctan-bis-mercury(II) Chloride The crystal structure of 1,8-dihydroxy-3,6-dithiaoctane-bis-mercury(II) chloride has been determined by X-ray crystal structure analysis. The compound crystallizes monoclinic, space group C2/c with a = 15.311(2), b = 5.870(2), c = 17.479(2) Å, β = 102.76° and 4 formula units per unit cell. The structure was solved by heavy atom technique and refined to a final R value of R = 0.050. Mercury is digonally coordinated by an S and a Cl ligator. In consequence of weak interactions to an oxygen atom of the ligand as well as to three further Cl ions the coordination number is increased to six and a strongly distorted octahedron is formed. The crystal structure is built up from polymeric complex molecules.     

Darstellung und Kristallstruktur von Rubidiumtrijodoplumbat(II)

Preparation and Crystal Structure of Rubidium Triiodoplumbate(II) RbPbJ₃ crystallizes in the orthorhombic space group Pnam(D) (lattice parameters see above); it is isomorphous with CsPbJ₃. The crystal structure has been determined from 1452 independent reflexes by Patterson- and Fourier-syntheses and refined three dimensionally by least-squares-methods. 6 I surround Pb nearly octahedrally. The octahedra are arranged in the form of double chains along the c-axis, which are held together by Rb. (Pb? I bond distances see above). The “inert 6s-pair” at Pb is stereochemically inactive.     

Fluorokomplexe von Platin(II): Synthese,NMR‐ und Schwingungsspektren von Tetrafluoroplatinat(II) und Difluorooxalatoplatinat(II)

Fluorine Complexes of Platinum(II): Synthesis, NMR and Vibrational Spectra of Tetrafluoroplatinate(II) and Difluorooxalatoplatinate(II) From the platinum(IV) compounds (n‐Bu₄N)₂[PtF₄(ox)] und cis‐(n‐Bu₄N)₂[PtF₂(ox)₂] on exposure to ultraviolet light at —196 °C the new platinum(II) fluorine complexes (n‐Bu₄N)₂[PtF₄] ( 1 ) and (n‐Bu₄N)₂[PtF₂(ox)] ( 2 ) are formed by elimination of a single oxalate ligand. With the synthesis of 1 the series of the tetra halogeno platinates(II) is completed now. With Cs⁺ and bis‐(triphenylphosphine)iminium(PNP⁺) as cations tetrafluoroplatinate(II) can be precipitated as pale yellow salts. Under exclusion of air all compounds are stable at —30 °C for several days, but they decompose and become black at room temperature in air within some hours. The infrared spectrum (60 K) of 1 exhibits the antisymmetric PtF stretching vibration at 515 and two deformation vibrations at 255 and 230 cm^—1. In the Raman spectrum (293 K) of (PNP)₂[PtF₄] the symmetric PtF stretching vibrations appear at 595 and 565 cm^—1. The calculated valence force constant is f_d(PtF) = 3.09 mdyn/Å. The NMR shifts are δ(¹⁹⁵Pt) = 6592 ( 1 ) and 5099 ( 2 ) and δ(¹⁹F) = —428 ( 1 ) and —393 ppm ( 2 ) with the coupling constants ¹J(PtF) = 1747 ( 1 ) and 1385 Hz ( 2 ).     

Darstellung und Eigenschaften von Kupfer(II)-Hypophosphit

Thermal Behaviour of the Mixtures Na₂S? P₄S₁₀ and Na₄Ge₄S₁₀? P₄S₁₀ of the System Na₂S? GeS₂? P₄S₁₀ The mixtures of Na₂S? P₄S₁₀ and Na₄Ge₄S₁₀? P₄S₁₀ were investigated by DTA and DSC. In the system Na₂S? P₄S₁₀ the congruently melting compounds Na₃PS₄ and (NaPS₃)_x and the peritectic phase Na₄P₂S₇ were found. The IR-spectra are given. Glassy, anhydrous and hydrated Na₄Ge₄S_l0 were prepared and thermochemically characterized. The section Na₄Ge₄S₁₀? P₄S₁₀ is not quasibinary, the mixed cage-anion Ge_4?xP_xS₁₀^(4?x)? thus cannot be prepared by heating and annealing mixtures of Na₄Ge₄S₁₀ and P₄S₁₀.     

Darstellung und Kristallstruktur von Blei(II)-monoglycerat

Preparation and Crystal Structure of Lead(II) Monoglycerolate Crystals of lead(II) monoglycerolate, of a quality suitable for diffraction studies, have been prepared from an alkaline plumbate solution and an excess of glycerol. The compound crystallizes in the monoclinic space group P2₁/c with a = 5.617(6) Å, b = 9.471(8) Å, c = 9.726(7) Å, β = 102.65(11)°. The structure was refined by full matrix least-squares techniques to an R value (1026 F₀) of 0.078. The compound to which the formula Pb(C₃H₆O₃) could be assigned, is polymeric in one direction. The lead and a part of the oxygen atoms built up a zig-zag chain parallel to the aaxis. The oxygen form a distorted tetragonal pyramid with lead at the apex. A decomposition temperature of 235°C has been determined.     

Synthese und Charakterisierung von Sulfinato-Nickel(II)-Komplexen

Synthesis and Characterization of Sulfinato-Nickel(II) Complexes Synthesis and properties of sulfinato-nickel(II) complexes of the type L₂Ni(Cl)SO₂R (L₂ = TMED, bipy, phen, DPPE, (PBu₃)₂; R = Ph, p-Tol, Me, NMe₂) are described. The compounds obtained are characterized by means of magnetic measurements, i.r. and reflectance spectra.     

Röntgenographische Untersuchungen und Strukturchemie von Chalkogenomolybdaten und -wolframaten. II

X-Ray Investigations and Structure Chemistry of Chalkogenomolybdates and -tungstates. II. The chalkogenomolybdates and -tungstates (NH₄)₂MoS₃Se, (NH₄)₂MoS₂Se₂, (NH₄)₂MoSSe₃, (NH₄)₂WSSe₃, Cs₂MoS₂Se, Cs₂MoS₂Se, Cs₂MoSSe₃, Cs₂WSSe₃, Cs₂MoOS₂Se, Cs₂WOS₂Se, Cs₂MoOSSe₂, and Cs₂WOSSe₂ are investigated by means of X-ray powder diffractometry. All compounds crystallize orthorhombic in spacegroup D? Pnma and are isomorphous with β-K₂SO₄. Systematic relations between lattice constants and occupation of atomic positions in the unit cell are discussed.     

Zur Analyse von Organozinnverbindungen und zur Reinheitskontrolle von Zinn(II)-salzen

Ohne Zusammenfassung     

Ueber die Farbe von Photochlorid und kolloidem Silber. II

Ohne Zusammenfassung Siehe Koll.-Zeitschr.28, 243 (1921). Auszug aus: Theodor Marx, Chemisches Verhalten und spektrale Eigenschaften von Silbersolen. Gie\ener Dissertation 1921.     

Synthese einiger Glucuronid-Metaboliten von Phenacetin und Phenetidin,Teil II

The anomeric configuration of the main metabolite of phenacetin, p-acetamido-phenyl β-D -glucopyranosido-uronic acid, was established by configurative correlation with a cyclohexyl β-D -glucopyranosido-uronic acid derivative. Furthermore, some anomeric D -gluco-pyranoside conjugates of 2-ethoxy-5-acetamido-phenol were synthesized and characterized using NMR.-spectroscopy and ORD./CD.