Ti7Cl16 und Ti7Br16 sowie weitere Untersuchungen mit Titanhalogeniden. Al2X6 als Komplexbildner

Ti₇Cl₁₆ and Ti₇Br₁₆ and Further Investigations with Titanium Halides. Al₂X₆ as a Complex Forming Agent TiCl_3,s can be transported with Al₂Cl₆ via TiAlCl_6,g in a temperature gradient. The equilibrium of this reaction was studied by mass spectroscopy. There is no indication of the existence of a TiAl₂Cl₉ molecule as assumed in the literature. β-TiBr₃ was prepared from the elements in the presence of the transporting agent Al₂Br_6,g. The transport of TiCl₂ with Al₂Cl_6,g involves, as an important step, the disproportionation which is favoured by the reaction of Ti with the glass wall. If the disproportionation is made impossible by addition of Ti the novel compound Ti₇Cl₁₆ is obtained. Independent of Ti₇Cl₁₆, a phase TiCl_{(2 + x)} with a broad range of homogeneity exists. The compound Ti₇Br₁₆, being isostructural with Ti₇Cl₁₆, was also prepared. Results of magnetic measurements and observations on the thermal decomposition of the compounds are reported.     

Magnetische Ordnungsphänomene in den Clusterverbindungen Ti7Cl16 und Ti7Br16

Magnetic Ordering Phenomena in the Cluster Compounds Ti₇Cl₁₆ and Ti₇Br₁₆ The magnetic susceptibilities of Ti₇Cl₁₆ and Ti₇Br₁₆ have been measured between 3.8 and 295 K by the Faraday method. The compounds show magnetic ordering points at 15.9 and 13.5 K, respectively. The determination of the oxidation states of the titanium ions and the exchange interactions between them is complicated by the fact that at room temperature competing antiferro-magnetic intra- and intercluster exchange interactions are already present. Calculations with simple models agree with the assumption that the compounds consist of Ti₃ clusters with Ti^II and isolated Ti^IV ions.     

Die KristallStruktur von LiAlCl4 · 3 SO2

Crystal Structure of LiAlCl₄ · 3 SO₂ Single crystals of LiAlCl₄ · 3SO₂ were grown on a 4-circle diffractometer in a temperature gradient 17°/40°C and diffraction data were collected at ?10°C. The compound crystallizes in the orthorhombic system, space group Pnam (No. 62) with a = 951.6(5), b = 1327.1(9), c = 1017.4(8) pm, Z = 4. The atomic parameters were refined to R = 0.049. The characteristic structural units are parallel strings of the composition Li(SO₂)_6/2. The spaces between these strings are occupied by nearly ideal tetrahedral AlCl₄ ions. The close relationship with the structure of LiClO₄ ·% 3H₂O is discussed.     

Die quantitative Bestimmung von Kohlenstoff und Wasserstoff in organischen Verbindungen mit Arsen und mit Quecksilber

Ohne Zusammenfassung     

Die Trennung schwelelhaltiger und schwefelfreier organischer Verbindungen mit Hilfe von Quecksilbersalzen

Ohne Zusammenfassung     

Die Bestimmung von Kohlenstoff und Wasserstoff in organischen Verbindungen mit einer schnellen gravimetrischen Mikromethode

Zusammenfassung Eine einfache gravimetrische Schnellmethode zur Mikrobestimmung von Kohlenstoff und Wasserstoff wird beschrieben. Die Probe wird im Luftstrom bei 1050 bis 1070° C vergast und über einer Kupferoxidschicht oxydiert. Die Stickoxide werden durch metallisches Kupfer reduziert. Die Gesamtdauer der Analyse beträgt 14 bis 16 Minuten.

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The determination of carbon and hydrogen in organic compounds by means of a rapid gravimetric micromethod

Summary A simple gravimetric rapid procedure is described for the microdetermination of carbon and hydrogen. The sample is gasified at 1050 to 1070° in a stream of air and oxidized over a copper oxide layer. The nitrogen oxides are reduced by metallic copper. The analysis consumes altogether 14 to 16 minutes.

     

Die Extrahierbarkeit von Alkaloiden und einigen anderen organischen Basen in Form von Verbindungen mit sauren Farbstoffen

Ohne Zusammenfassung     

Die Kristallstruktur der Verbindungen BaCaGaF7 und BaCaCrF7

Crystal Structure of the Compounds BaCaGaF₇ and BaCaCrF₇ The isostructural fluorides BaCaGaF₇ and BaCaCrF₇ (values in parentheses) crystallize monoclinically in space group P2/n, Z = 4: a = 539.0 (539.8), b = 541.0 (542.2), c = 1897.8 (1900.6) pm, β = 92.33 (92.10)°. Complete X-ray single crystal structure determinations showed, that the compounds are built up from triple layers [CaF_8/2 · MF₃]^2?, which consist of a central sheet of edge-sharing CaF_8/2^2? polyhedra (distorted square antiprisms) with M^IIIF₆octahedra condensed on it at both sides and which are held together by 12-coordinated barium ions. The resulting average distances are: Ga? F = 187.8 (Cr? F = 189.4) pm, Ca ? F = 236.2 (236.2) pm, Ba? F = 289.4 (289.4) pm. Some relations to the structures of other fluorides are discussed.     

Die Spektralanalyse von Bleiglas auf F, Cl und As mit der Hohlkathodenentladung

Ohne Zusammenfassung     

Die Mikrobestimmung von C und H borhaltiger Verbindungen

Ohne Zusammenfassung     

Die Kristallstruktur von Ti3InC,Ti3InN,Ti3TIC und Ti3TIN

Zusammenfassung Die ternären Phasen Ti₃InC, Ti₃InN, Ti₃TIC und Ti₃TIN werden aus TiC (TiN) und den metallischen Komponenten hergestellt. Diese Verbindungen sind mit den Perowskit-Carbiden (-Nitriden) isotyp.     

Die Schichtstruktur von Cyamelurchlorid C6N7Cl3

The Layer Structure of Cyameluric Chloride C₆N₇Cl₃ A solid state reaction of cyanuric chloride (trichloro‐s‐triazine C₃N₃Cl₃) with sodium dicyanamide (NaN(CN)₂) yielded some yellow, plate‐like crystals of cyameluric chloride (trichloro‐s‐heptazine C₆N₇Cl₃). The crystal structure was determined by single crystal X‐ray diffraction at 220 K and was solved in the monoclinic space group C 2/c (no. 15) with Z = 24, a = 2319.4(4) pm, b = 1348.8(1) pm, c = 2063.4(3) pm, β = 118.38(2)° and V = 5.680(1) nm³. In the structure, the molecules of C₆N₇Cl₃ are forming layers parallel to the ab‐plane, which are separated from each other by a gap of approximately 300 pm. In each of these layers, the molecules seem to be arranged around pseudo‐threefold axes, showing an almost trigonal structure pattern.     

Die Photoionenspektren von SCl2, S2Cl2 und S2Br2

Photoionization Mass Spectra of SCl₂, S₂Cl₂, and S₂Br₂ Photoionization mass spectra of SCl₂, S₂Cl₂, and S₂Br₂ have been measured. Heats of formation, bond energies, and ionization potentials of fragments have been calculated from appearance potentials.     

Die Ultraviolettabsorption von organischen Peroxyden und verwandten Verbindungen

Zusammenfassung Es wird die Ultraviolettabsorption (in Benzinlösung im Bereich bis ungefähr 2200 ) von Benzoylperoxyd, o- und p-Toluylperoxyd, o-, o- und p-, p-Dichlorbenzoylperoxyd, Cinnamoylperoxyd, Tetralinhydroperoxyd, Benzoesäureanhydrid, o- und p-Toluylsäureanhydrid, Zimtsäureanhydrid gemessen.In dem untersuchten Bereich liefert die –O–O-Gruppe praktisch keinen Beitrag zur Lichtabsorption.Mit 5 Abbildungen.