FG Anorganische Chemie - Festkörper- und Materialchemie

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Verteilung und Valenz der Kationen in Spinellsystemen mit Eisen und Vanadium, I Röntgenographische und Mößbauer-spektroskopische Untersuchung des Spinellsystems ZnV2O4-ZnFe2O4

Riedel, Erwin ; Dützmann, Till ; Pfeil, Norbert (1980)

The spinel system Zn[FexV2-x]O4 has been prepared by heating mixtures of ZnV2O4 and ZnFe2O4 at 1000 °C. The lattice constants increase linearly with x by 3.6 pm, the oxygen parameters are constant with a mean value u = 0.384s. The parameters of room temperature Mössbauer spectra show that in the whole series V(III) and Fe(III) are present.

Verteilung und Valenz der Kationen in Spinellsystemen mit Eisen und Vanadium, II Röntgenographische Untersuchung, Seebeck Koeffizienten, Mößbauer-und IR-Spektren der Mischkristallreihen Fe2VO4-ZnV2O4 und Fe2VO4-ZnFe2O4

Riedel, Erwin ; Pfeil, Norbert (1980)

The spinel series Fe2VO4-ZnV2O4 and Fe2VO4-ZnFe2O4 have been prepared and investigated. The lattice constants and Mössbauer spectra lead to a distribution of cations which proves that Fe2VO4 is a partially inverse spinel with Fe(II) and Fe(III) on the tetrahedral site. The Seebeck effect is interpreted with a model of both tetrahedral and octahedral conduction based on charge hopping.

Röntgenstrukturanalyse und Schwingungsspektren von Trischwefeldistickstoffdioxid, S3N2O2 [1]

Steudel, Ralf ; Steidel, Jürgen ; Rautenberg, Norbert (1980)

A redetermination of the crystal and molecular structure of the chain-like molecule S(NSO)2 resulted in the following molecular parameters: d(SO) = 146.5(2), d(S = N) = 153.4(2), d(S-N) = 165.7(2) pm, bond angles OSN = 117.5(1)°, SNS = 123.6(2)°, and NSN = 97.2(1)°, torsion angles OSNS = -0.3(2)°, and SNSN = -177.7(2)° (molecular symmetry C2). Infrared and Raman spectra of S(NSO)2 are reported ...

Di-μ-iodo-bis [dicarbonyl(di-tert-butylphosphin)ruthenium(I)] (Ru-Ru) und Bis(tri-tert-butylphosphonium)-di-μ-iodo-bis[carbonyl-diiodo- (di-tert-butylphosphin)ruthenium(II)]

Schumann, Herbert ; Opitz, Joachim (1980)

[(t-C4H9)3PH]2[{Ru(μI)I2(CO)[P(t-C4H9)2H]}2] is prepared by the reaction of RUC13 · (H2O)x with CO, NaI, and P(t-C4H9)3 in 2-methoxyethanol. Its IR, Raman, and NMR spectra are reported and discussed. [Ru(μ-I)(CO)2P(t-C4H9)2H)2 is obtained by the reaction of [Ru(μ-I)I(CO)3]2 with P(t-C4H9)3 in 2-methoxyethanol. The X18MAA′M′X′18 spin system of its 1H NMR spectrum is analysed.

Verteilung und Valenz der Kationen in Spinellsystemen mit Eisen und Vanadium, III Röntgenographische und Mößbauer-spektroskopische Untersuchung des Spinellsystems ZnFeVO4-Fe3O4

Riedel, Erwin ; Anik, Hümeyra ; Dützmann, Till (1981)

The spinel system Zni_zFe2:[Fei+2;Vi_I]04 has been prepared by heating mixtures of ZnFeV(>4 and Fe3Ü4 at 1000 °C. The lattice constants, the oxygen parameters and the Mössbauer parameters show that a transition from a nearly normal to an inverse distribu-tion of Fe(II) and Fe(III) exists.

Nachweis von Se6, Se7 und Se8 in Lösungen yon Selen mittels Hochdruckflüssigkeitschromatographie

Steudel, Ralf ; Strauss, Eva-Maria (1981)

Dissolution of crystalline Se8 or extraction of glassy or red amorphous selenium, prepared from aqueous SeO2 by reduction, by organic solvents yields solutions containing Se6, Se7 and Se8 in equilibrium as shown by HPLC. The equilibrium explains the concentration dependence of the molar absorbance of such solutions observed earlier. Since the Raman spectrum of red amorphous selenium does not sh...

Metallkomplexe mit Hexamethylentetramin als Ligand: Kristallstruktur des Cadmiumiodid-Addukts 3Cdl2 • 2 C6H12N4 • 4 H2O

Pickardt, Joachim (1981)

The reaction of aqueous solutions of cadmium iodide and hexamethylenetetramine yields crystals of an adduct 3CdI2 • 2CeH12N4 • 4H2O. The crystals are monoclinic, space group P 21/n, Z = 2, a = 811.5(2), b = 1049.2(4), c = 1849.5(6) pm, β = 97.73(2)°. The adduct is polymeric and may be regarded as built up from groups of two tetrahedrally and one octahedrally coordinated Cd(II) ions in which the...

Nachweis der re-entrant nematischen Phase an verschiedenen homologen biaromatischen Flüssigkristallen durch Untersuchung binärer Mischsysteme

Göbl-Wunsch, A. ; Heppke, G. ; Hopf, R. (1981)

Several homologous series of biaromatic liquid crystals with structure type CnH2n+1O • C6H4 • M•C6H4-CN are investigated. By studying the phase transition temperatures in binary mixed systems a "re-entrant" nematic phase N(re) is established for all compounds exhibiting smectic A phases. The virtual transition temperatures N(re) - SA are found to decrease with increasing chain length of the alk...

Vibrational Spectra and Force Constants of Tetrasulfurtetranitride, S4N4 [1]

Steudel, Ralf (1981)

Infrared and Raman spectra of solid and dissolved S414N4 and of solid S415N4 have been recorded and assigned in accordance with the molecular point group D2d. 22 of the 28 fundamental vibrations of both molecules have been identified and used to calculate force constants applying a modified Urey-Bradley force field with 9 independent constants. Good agreement between observed and calculated wav...

Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2

Köpf, Hartmut ; Pickardt, Joachim (1981)

The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titan...

Entropies and Heat Capacities of Gaseous Selenium Molecules Sen (n = 5 ... 12)

Steudel, Ralf (1981)

Thermodynamic functions are calculated for gaseous Se8 molecules from spectroscopic and structural data and listed for temperatures up to 3000 K. Entropy (S°) and heat capacity (Cp0) data for Sen molecules (n = 5, 6, 7, 9, 10, 11, 12) are obtained from linear relationships between both S0 and Cp0 and ring size n which are derived from the corresponding values of Se2 and Se8.

Metallorganische Verbindungen der Lanthanoiden, XTTT [1] Tris(di-f-butylarsin)-Derivate von Yttrium, Lanthan, Praseodym, Holmium, Erbium, Thulium und Lutetium

Schumann, Herbert ; Frisch, Georg-Michael (1982)

Lithium (di-t-butyl) arsenide reacts with the trichlorides of yttrium, lanthanum, praseodymium, holmium, erbium, thulium, and lutetium under elimination of lithium chloride and formation of the corresponding tris(di-t-butylarsine) derivatives.

Equilibria between Sulfur Rings in Carbon Disulfide Solution at Elevated Temperatures

Steudel, Ralf ; Strauss, Reinhard (1982)

Cyclooctasulfur, S8, dissolved in CS2 reacts at 130-155 °C in sealed ampoules to give S6 and S7 whose concentrations have been determined by HPLC. The half-time of the reaction is independent of the initial S8 concentration and decreases from 232 min at 130 °C to 64 min at 150 °C. After long reaction times equilibrium concentrations are observed which are in agreement with the law of mass actio...

Die Kristallstruktur von Hexa-μ-chloro-μ4- oxo - tetrakis [hexamethy lentetramin - kupfer(II)] , [CU4Cl60(C6H12N4)4] , einem Kupfer(II)-Komplex mit Berylliumoxoacetat-ähnlicher Struktur

Pickardt, Joachim ; Rautenberg, Norbert (1982)

By reaction of solutions of CuCl2·2H2O and hexamethylenetetramine, C6H12N4, in acetone, a complex [Cu4Cl6O(C6H12N4)] could be obtained as single crystals. An X-ray analysis shows that the complex has a structure related to that of basic beryllium acetate. An oxygen atom is tetrahedrally surrounded by four cop-per atoms which, together with six chlorine atoms, form an adamantane-like core. Each ...

Metallkomplexe mit Hexamethylentetramin als Ligand, VI [1] Kristallstruktur von Bis-hexamethylentetramin-bisisocyanatokupfer(II), [CU(NCO)2(C6H12N4)2]hexamethylenetetramine-bisisocyanatocopper(II), [Cu(NCO)2(C6Hl2N4)2]

Pickardt, Joachim ; Rautenberg, Norbert (1982)

Crystals of the complex [Cu(NCO)2(C6Hi2N4)2] could be obtained by reaction of copper- (II)nitrate, hexamethylenetetramine, and KNCO in CHCI3 as a solvent. The crystals are triclinic, space group Cl, Z = 4, a = 1373.1(9), b = 2083.1(9), c = 642.6(3) pm, a = 91.05(4), β = 90.54(6), y = 107.39(6)°. The copper atom is bonded to two terminal cyanato groups via the nitrogen atoms, and to two liexamet...

Verteilung und Valenz der Kationen in Spinellsystemen mit Eisen und Vanadium, IV. Rontgenographische und Mößbauer-spektroskopische Untersuchung des Spinellsystems FeV2O4-ZnV2O4

Riedel, Erwin ; Anik, Hümeyra (1983)

In the spinel system FeV2O4-ZnV2O4 pure Fe(II)-spinels could not be prepared. Mössbauer spectra show that the solid solution has the composition Fex2+ Zn1-x:[Fey3+ V2-y]O4, y depending on the partial pressure of oxygen during preparation. The reaction of 1/3 Fe + 1/3 Fe2O3 + V2O3 in a closed tube was also studied by X-ray and Mössbauer investigation.

Barrier to Rotation about Sulfur-Sulfur Bonds in Homocyclic Sulfur Molecules

Steudel, Ralf (1983)

It is shown that the distances (d) of the 19 longest bonds in 9 homocyclic sulfur rings of type Sn (n = 6-20) depend on the torsional angles (τ) which vary between 0° and 140°. The function d = f(τ) is smallest for τ = 90-100° and largest for τ = 0°; the corresponding bond distance variation amounts to 13 pm or 6%. The height of the torsional cis-barrier is estimated from the enthalpy of format...

Chromatographische Trennung schwefelhaltiger Heterocyclen der Typen (CH2)nSm und SenS8-m mittels HPLC [1]

Steudel, Ralf ; Strauss, Eva-Maria (1983)

The Separation of a number of cyclic methylene sulfides and selenides by reversed-phase high-pressure liquid chromatography is reported. The retention times as well as the capacity factors depend in a systematic way on the ring size, the number and kind of chalcogen atoms, and the number of heteronuclear bonds within the ring. These relation-ships are used to assign the chromatograms of cyclic ...

X-Ray Structural Analyses of Cyclodecasulfur (S10) and of a Cyclohexasulfur-Cyclodecasulfur Molecular Addition Compound (S6 · S10) [1]

Steudel, Ralf ; Steidel, Jürgen ; Reinhardt, Richard (1983)

Low temperature X-ray structural analyses of monoclinic single crystals of S10 and S6 · Si10 (prepared from the components) show that the cyclic S10 molecule exhibits the same D2 conformation in both compounds with bond distances between 203.3 and 208.0 pm, bond angles (α) between 103 and 111°, and torsional angles (τ) between 73 and 124°. The S6 molecule (site symmetry Ci) in S6 · S10 is very ...

Synthese und Eigenschaften von TrimethyIstannylmethyl-Indium(III)-Verbindungen

Schumann, Herbert ; Mohtachemi, Reza (1984)

Trimethyltin methyllithium reacts with InCl3, CH3InCl2 and R2InCl (R = CH3, t-C4H9) with formation of the new compounds In(CH2SnMe3)3, CH3In(CH2SnMe3)2, (CH3)2InCH2SnMe3 and (t-C4H9)2InCH2SnMe3. The compounds are characterized by elemental analyses, 1H, 13C, 119Sn NMR and IR spectra.