Published by De Gruyter

Volume 48 Issue 5

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Na₂TiOS₂ — Ein Oxothiotitanat(IV) mit unendlichen Tetraederketten / Na₂TiOS₂ — An Oxothiotitanate(IV) with Infinite Tetrahedral Chains

O. Klepp

Page range: 545-547

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Abstract

Colourless single crystals of Na 2 TiOS 2 were obtained by a fusion reaction of a stoichiometric mixture of Na 2 S, Na 2 SO 3 , titanium-powder and elemental sulphur. Na 2 TiOS 2 is monoclinic, space group P2 1 /c with a = 6.861(3), b = 13.610(9), c = 5.733(9) Å, β = 113.24(2)°, Ζ = 4. The crystal structure (R = 0.032, 811 observations, 55 variables) is characterized by infinite anionic chains of TiO 2 S 2 -tetrahedra sharing the oxygen atoms (d̄ Ti-o = 1.842 Å, d̄ Ti-s = 2.227 Å, Ti—O—Ti = 134.3°). The chains are separated from each other by octahedrally coordinated Na + ions. The structure may be considered as a quaternary variant of the Na 2 GeS 3 -structure type.

Open Access June 2, 2014

Clusterdithiophosphinate mit kubanartigem Mo₂M₂S₄-Kern (M = Co, W) / Clusterdithiophosphinates with Cubane-Type Mo₂M₂S₄-Core (M = Co, W)

Hansjörg Diller, Helmut Keck, Andreas Kruse, Wilhelm Kuchen

Page range: 548-554

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Abstract

The syntheses of tetranuclear complexes Mo,W 2 S 4 L 6 3 and Mo 2 Co 2 S 4 L 2 (CO) 2 (CH 3 CN) 2 4 (L = R 2 PS 2 ⁻; a: R = Et, b: R = Pr) containing the cubane-type Mo 2 M 2 S 4 core are reported. While in 4 both Mo atoms are chelated by L, the dithiophosphinato group acts as a chelating and bridging ligand in 3. It is shown that there exist four isomers of 3 which differ not only in the function of L but also in the kind of metals which are chelated and bridged. Magnetic and NMR spectroscopic data are given. The structure of a mixed crystal of the two β-isomers of 3a containing three bridging and three chelating ligands L is reported: orthorhombic space group Pbca, Z = 8, and lattice parameters a = 2186.6(7), b = 2264.0(7), and c = 2386.7(6) pm.

Open Access June 2, 2014

X-Ray Structural Analysis and Vibrational Spectra of Sodium Cysteine-S-sulfonate, ⁺H₃NCH(COO-)CH₂S₂O₃Na • 3/2H₂O [1]

Ralf Steudel, Angela Albertsen, Monika Kustos, Joachim Pickardt

Page range: 555-560

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Abstract

The title compound crystallizes orthorhombically (space group C 222 1 ) with a = 797.0, b = 870.3 and c = 2739.0 pm. The anions are zwitterions which are heavily involved in intra- and intermolecular NH •••O and OH•••O hydrogen bonding. The two types of sodium cations are coordinated by six oxygen atoms each of which belongs to either SO 3 groups (Na 2) or water molecules and SO 3 groups (Na1). A second type of water molecules is not coordinated to the cations. The SS bond length is 208.2 pm. Infrared and Raman spectra of the title compound are reported and tentatively assigned. The SS stretching vibration is observed at 409 cm -1 .

Open Access June 2, 2014

Reaktionen von Pyridin-Basen mit Na/K-Legierung und Diorganylaminodifluorboranen / Reactions of Pyridine-Bases with Na/K-Alloy and Diorganylaminodifluoroboranes

Walter Maringgele, Anton Meller, Sven Dielkus, Regine Herbst-Irmer

Page range: 561-570

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Abstract

Lutidines react with Na/K alloy and diorganylaminodifluoroboranes in n-hexane. The products formed depend upon the position of the methyl groups. While from 3,4-lutidine (C) the bis(lutidinyl)aminoboranes 2 - 5 are obtained, the 2,4-, 2,5-, and 3,5-lutidines (F, G, H) give the 11 a, 1 lb-dihydro-[1,3,2]-diazoborolo-[5,l-b;3,4-b']-dilutidines 11-17. 4-Picoline reacts analogously to give 10. Pyridine (A) and collidine (B) give adducts with borane. From 2,3-lutidine (D), the 1,4-dihydro-l,4-bis(fluoraminoboryl)-2,3-lutidine 8 is obtained. 1 H, 11 B, 13 C, 19 F, 29 Si, 15 N NMR and MS data are given. For 8 and 14 the X-ray structures are reported.

Open Access June 2, 2014

Addukte Aromat/Chlorwasserstoff bei tiefen Temperaturen: Beiträge zu Bildung und Kristallstruktur [1] / Adducts Arene/Hydrogen Chloride at Low Temperatures: Contributions to Formation and Crystal Structure [1]

Axel Deeg, Dietrich Mootz

Page range: 571-576

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Abstract

The melting diagrams of the systems benzene-HCl, toluene-HCl and mesitylene-HCl have been established and the crystal structures of two adducts determined. The adduct toluene · 2 HCl, melting incongruently at -115°C, is monoclinic with space group C2/c and Ζ = 4 formula units per unit cell; the adduct mesitylene · HCl, m. p. -64°C, is orthorhombic with space group Pbca and Ζ = 8. The HCl molecules are situated on both sides and one side, respectively, of the plane of the aromatic system and are linked to it by weak hydrogen bonds of the type Cl-H···π.

Open Access June 2, 2014

Oligophosphan-Liganden, XXXVIII / Oligophosphine Ligands, XXXVIII

Darstellung, Isomerie und Reaktivität von Arylhydridoruthenium(II)-Komplexen [MeSi(CH₂PMe₂)₃l(Me₃P)RuH(Ar) / Preparation, Isomerism, and Reactivity of Arylhydridoruthenium(II) Complexes [MeSi(CH₂PMe₂)₃](Me₃P)RuH(Ar)

Corinna Becker, Lutz Dahlenburg, Sabine Kerstan

Page range: 577-582

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Abstract

Intermolecular activation of carbon-hydrogen bonds has been accomplished by reduction with sodium amalgam of (sip 3 )(Me 3 P)RuCl 2 , 1, [“sip 3 ” = MeSi(CH 2 PMe) 2 ) 3 ] in aromatic hydrocarbons, such as benzene and substituted derivatives thereof. In these reactions, the 16e equivalent (sip 3 XMe 3 P)Ru(O) thus generated exhibits a preference for insertion across the unhindered metaand para-C-H bonds to produce complexes of composition (sip 3 )(Me 3 P)RuH(C 6 H 3 RR′) [R = R′ = H, 2; R = H, R′ = CH 3 , 3; R = R′ = CH 3 (3,4-xylyl), 4; R = R′ = CH 3 (3,5-xylyl), 5; R = H, R′ = CF 3 , 6], of which 3, 4, and 6 were isolated as mixtures of meta/para-isomers and Ru-aryl rotamers, respectively. Reaction of the phenyl hydride 2 with 4-MeC 6 H 4 NCE (E = O, S) leads to insertion of the heteroallenes into the Ru-Η bond to give (sip 3 )(Me 3 P)Ru[N(C 6 H 4 Me-4)C(O)H]C 6 H 5 , 8, and (sip 3 )(Me 3 P)Ru[SC(=NC 6 H 4 Me-4)H]C 6 H 5 , 10, as the primary products. While the latter forms (sip 3 ), 11, by loss of PMe 3 , the former reacts with another molecule of isocyanate to afford the acyl compound (sip 3 )9, as the ultimate product. Treatment of 2 with CO 2 results in the formation of a carbonato derivative, (sip 3 )(Me 3 P)Ru(O 2 CO), 7. •

Open Access June 2, 2014

Koordinationschemie perhalogenierter Cyclopentadiene und Alkine, XI [1].<br />Darstellung einiger Cymantrenyl-mono- und bis-thioether mit einer weiteren funktionellen Gruppe am Cyclopentadienylring. Molekülstruktur von [C₅Cl₂(SMe)₂(PPh₂)]Mn(CO)₃ / Coordination Chemistry of Perhalogenated Cyclopentadienes and Alkynes, XI [1]<br />Synthesis of Some Cymantrene Mono- and Bis-Thioethers with One Additional Functional Group on the Cyclopentadienyl Ring. Molecular Structure of [C₅Cl₂(SMe)₂(PPh₂)]Mn(CO)₃

Karlheinz Sünkel, Adrian Blum, Barbara Wagner

Page range: 583-590

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Abstract

Chiral Cyclopentadienyl Complexes, Crystal Structure The reaction of [C 5 Cl 4 (SMe)]Mn(CO) 3 (la) with n-butyllithium and the electrophiles SiMe 3 Cl, CO 2 , or PPh 2 Cl regiospecifically yields the chiral 1,3-disubstituted functional cymantrene thioethers [C 5 Cl 3 (SMe)R]Mn(CO) 3 (R = SiMe 3 (2), COOLi (3a), PPh 2 (4)). 3 a can be protonated to give the corresponding carboxylic acid (3b), which in turn can be transformed to the acid chloride [C 5 Cl 3 (SMe)(COCl)]Mn(CO) 3 (3c). 3c reacts with NaN 3 to yield after work-up the urea derivative OC[[NH—C 5 Cl 3 (SMe)]Mn(CO) 3 ] 2 (3d). Using the cymantrene bisthioethers [C 5 Cl 3 (SR) 2 ]Mn(CO) 3 (R = Me, 5a, Ph, 5b) as starting materials, the carboxyl derivatives [C 5 Cl 2 (SMe) 2 (COR)]Mn(CO) 3 (R = OLi, 6a, OH, 6b, Cl, 6c) and the potential organometallic S,P-chelate ligands [C 5 Cl 2 (SR) 2 (PPh 2 )]Mn(CO) 3 (R = Me, 7a, Ph, 7b) can be obtained. The crystal structure determination of 7a (C 22 H 16 O 3 PS 2 Cl 2 Mn, monoclinic, P 2 1 /c, a = 18.714(6) A, b = 9.506(3) A, c = 14.475(3) Α, β = 109.18(2)°, V = 2432.1(12) Α 3 , Z = 4) shows an orientation of the neighbouring PPh 2 - and SMe groups, that allows chelation of an additional metal fragment.

Open Access June 2, 2014

Syntheses and Structures of Three Mononuclear Coordination Compounds Containing Six- and Seven-Coordinated Manganese(II) Ions

Marius Andruh, Kay Hübner, Mathias Noltemeyer, Herbert W. Roesky

Page range: 591-597

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Abstract

The reactions of Mn(CF 3 COO) 2 (1) with Ν,Ν,N′,N′-tetramethylethylenediamine (tmen), 2,2′-bipyridine (bipy) and triethanolamine (tea) yield three new mononuclear coordination compounds: trans-[Mn(tmen) 2 (CF 3 COO) 2 ] (2), cis-[Mn(bipy) 2 (CF 3 COO) 2 ] (3), and [Mn(tea)2](CF 3 COO) 2 (4). The X-ray structures of the compounds 2, 3, and 4 are described. The seven-coordination of the manganese(II) ion in 4, as well as the inequivalency of the two tea molecules coordinated to Mn(II) make this compound unique.

Open Access June 2, 2014

Darstellung, ¹¹B-, ¹³C-NMR- und Schwingungsspektren der closo-Hexaborate [B₆H₅(CN)1²- und cis-[B₆H₄(CN)₂]²⁻ sowie Kristallstruktur von Cs₂[B₆H₅(CN)] / Preparation, ¹¹B,¹³C NMR and Vibrational Spectra of the closo-Hexaborates [B₆H₅(CN)]^2- and cis-[B₆H₄(CN)₂]²-, and the Crystal Structure of Cs₂[B₆H₅(CN)]

W. Preetz, A. Franken, M. Rath

Page range: 598-602

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Abstract

By reaction of Cs 2 [B 6 H 6 ] with in situ generated dicyanogen in aqueous alkaline solution the monocyanohydrohexaborate Cs 2 [B 6 H 5 (CN)] and the dicyanohydrohexaborate cis-Cs 2 [B 6 H 4 (CN)2] are formed. The compounds have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of Cs 2 [B 6 H 5 (CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P2 1 /a with a = 9.540(8), b = 9.977(3), c = 10.578(2)Å, β = 105.06(2)°. The B 6 octahedron is compressed in the direction of the nearly linear B—CN bond by about 5%, with bond lengths between 1.71 and 1.76Å. The "B NMR spectra of the two compounds reveal the features of substituted B 6 cages with C 4v and C 2v point symmetry. In the 13 C NMR spectrum of Cs 2 [B 6 H 5 (CN)] a quartet at -139 ppm with 1 J(C,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs 2 [B 6 H 5 (CN)] at 2149, and for cis-Cs 2 [B 6 H 4 (CN) 2 ] at 2170 cm -1 .

Open Access June 2, 2014

Titan(IV)-Fulvalenkomplexe. Darstellung und Struktur von [CpTiPh₂l₂(C₁₀H₈) / Titanium(IV) Fulvalene Complexes. Preparation and Structure of [CpTiPh₂]₂(C₁₀H₈)

Ulf Thewalt, Thomas Wöhrle

Page range: 603-607

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Abstract

The green insoluble Ti IV compound which is obtained by treating titanocene with HC1 reacts with PhLi to yield the fulvalene-bridged compound [CpTiPh 2 ] 2 (C 10 H g ) 3(Ph). An X-ray structure analysis of 3(Ph) shows, that the Ti atoms are in a trans arrangement with respect to the fulvalene group. Crystal data for 3(Ph) are as follows: C 44 H 38 Ti 2 , orthorhombic, space group P2 1 2, 1 2 1 , with a = 11,385(2), b = 14,510(2), c = 19,489(4) Å, Z = 4. The crystals exhibit enantiomorphism.

Open Access June 2, 2014

Bis(di-tert-butylphosphino)ethan-nickel(0)-Komplexe / Bis(di-tert-butylphosphino)ethane-nickel(0) Complexes

Klaus-Richard Pörschke, Christian Pluta, Bernd Proft, Frank Lutz, Carl Krüger

Page range: 608-626

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Abstract

Ni(cdt) reacts with t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 in pentane at 20°C to yield brownish crystals of ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(η 2 -C 12 H 18 ) (1). The molecular structure of 1, as established by X-ray crystallography, exhibits a trigonal-planar coordination geometry of the nickel center with a η 2 bonded cdt ligand. In the crystal 1 exists as two enantiomers, which are determined by the leftor right-handed screw axis of the cdt ligand. The cdt ligand in 1 resists most typical displacement reactions but 1 reacts with CO at – 78°C to afford the colorless 18e complex ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(CO) 2 (2). From the reaction of Ni(cod) 2 with t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 yellow needles of ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(η 2 -cod) (3) are obtained. Low temperature NMR spectroscopy established that only one diene C=C bond is coordinated to nickel(0). At higher temperatures a rapid exchange of the coordinated and unbound C=C bonds is induced. When solutions of 3 are kept at 20°C for several days the dinuclear, almost insoluble yellow complex {( t Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni} 2 (μ-η 2 ,η 2 -cod) (4) precipitates. The reaction of Ni(C 2 H 4 ) 3 and t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 affords orange ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(C 2 H 4 ) (5). From Ni(1,5-hexadiene) 2 and t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 in 1,5-hexadiene the yellow-greenish complex ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(η 2 -C 6 H 10 ) (6) is obtained. As for 3, only one diene C=C bond is coordinated to nickel(0), but the structure is fluxional with exchange of the coordinated and unbound C=C bonds (NMR at 20°C). From a solution of 6 in pentane the dinuclear, diastereomeric compounds rac/meso-{( t Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni} 2 (μ-η 2 ,η 2 -C 6 H 10 ) (7a,b) separate in large yellow crystals. In similar reactions the 1,6-heptadiene complexes ( t Bu 2 Bu 2 PC 2 H 4 P t Bu 2 )Ni(η 2 -C 7 H 12 ) (8) and rac/meso-{( t Bu 2 Bu 2 PC 2 H 4 P t Bu 2 )Ni}2(µ-η 2 μ-η 2 ,η 2 -C 7 H 12 ) (9a,b) are also obtained. In 6, 7a,b, 8, and 9a,b the open-chain diene ligands can easily be displaced, e.g., by ethene to afford 5. Thus, complexes 6, 7a,b, 8, 9a, b are the most reactive. These complexes react readily (the ethene derivative 5 also reacts but very slowly) with butadiene to yield large yellow cubes of ( t Bu 2 Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(η7 2 -C 4 H 6 ) (10), which is also fluxional. The alkene complexes 5, 6, 7a, b, 8, 9a,b, 10 react with ethyne to yield yellow-brownish crystalline ( t Bu 2 t Bu 2 PC 2 H 4 P 4 P'Bu 2 )Ni(C 2 H 2 ) (11).

Open Access June 2, 2014

Metallkomplexe mit funktionalisierten Schwefelliganden, V Ruthenium(II)-Alkyl- und -Arylthiosulfinato-Komplexe. Kristallstrukturanalyse von CpRu(PPh₃)(CO)[S-S(O)-CH₂-C₆H₅] / Metal Complexes of Functionalized Sulfur Containing Ligands, V Ruthenium(II)-Alkyl-and -Arylthiosulfinato Complexes. X-Ray Structure Determination of CpRu(PPh₃)(CO)[S-S(O)-CH₂-C₆H₅]

Wolfgang Weigand, Gabriele Bosl, Christian Robl, Jürgen Kroner

Page range: 627-635

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Abstract

Compounds of the type CpRu(PPh 3 )(L)(SH) [L = PPh 3 (2), CO (4)] react with N-alkyl and -arylsulfinyl phthalimides 3a-f to give the chiral complexes CpRu(PPh 3 )(L)[S-S(O)-R] (L = PPh 3 , 5a: R = C 4 H 9 ,5b: R = C 12 H 25 ,5d: R = C 18 H 37 ,5e: R = Tol; L = CO, 6a: R = C 4 H 9 ,6b: R = C 12 H 25 ,6c: R = C 16 H 33 ,6d: R = C 18 H 37 ,6f: R = CH 2 Ph). With 6a-c diastereoselectivities of 5:2, with 6d 5:1, and with 6f 10:3, respectively, are observed. The compounds 5,6 are characterized by their spectroscopic data; the X-ray structural determination of u-6f shows a sulfur-sulfur bond length of 208,6 (3) pm, the dihedral angle Ru-S(1)-S(2)-C(25) is 170,8°. Extended Hückel calculations give information about the rotational barrier around the S-S(O) axis.

Open Access June 2, 2014

Darstellung und Eigenschaften von CH₃C(CH₂PPh₂)₃MoCl3 / Characterization and Properties of CH₃C(CH₂PPh₂)₃MoCl3

Olaf Walter, Gottfried Huttner, Laszlo Zsolnai

Page range: 636-640

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Abstract

Starting from MoCl 5 via the intermediates (MeCN) 2 MoCl4 (1) and (THF) 2 MoCl 4 (2) the tripod complex CH 3 C(CH 2 PPh 2 ) 3 MoCl 3 (4) has been synthesized. The yellow cristalline compound 4 has been fully characterized by standard analytical techniques. X-ray-analysis proves the facial coordination of the tripod ligand. To our knowledge 4 is the first Mo(III)-trihalide coordination compound containing three P-donor-ligands in a facial coordination.

Open Access June 2, 2014

Fünffach koordinierte Co(III)-Komplexe [Tripod-Cobalt-(ortho(X)(Y)C₆H₄)]⁺ mit ortho-phenylenverbrückten Chelatliganden [(XH)(YH)C₆H₄] (XH, YH = NH₂, OH, SH) / Five-Coordinate Co(III) Complexes [Tripod-Cobalt-(ortho-(X)(Y)C₆H₄)]⁺ Containing ortho-Phenylene-Bridged Chelate Ligands [(XH)(YH)C₆H₄] (XH, YH = NH₂, OH, SH)

Sabine Vogel, Gottfried Huttner, Laszlo Zsolnai

Page range: 641-652

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Abstract

The ortho-phenylene compounds ortho-[(XH)(YH)C 6 H 4 ] (XH, YH = NH 2 , SH, OH) react with Co(BF 4 ) 2 •6H 2 O and Tripod (CH 3 C(CH 2 PPh 2 ) 3 ) to give the five-coordinate Co(III) complexes [Tripod-Cobalt-(ortho-(X)(Y)C 6 H 4 )] + (X, Y = NH, O, S), 1-6. The structures of 1—6 have been characterized by X-ray analyses of appropriate salts. The compounds have further been characterized by IR, NMR, UV-VIS and cyclovoltammetric measurements. As a compound analogous to 1—6, but containing the saturated chelate ligand [(S)C 2 H 4 (S)] 2- instead of the conjugated ortho-phenylene type ligands of 1-6, [Tripod-Cobalt-((S)C 2 H 4 (S))] + , 7, has been prepared and fully characterized. It is inferred that the coordination geometries of 1-7 do not strongly depend on conjugative interaction within the chelating ligands.

Open Access June 2, 2014

N-Methylimidazole Mediated Chemistry of Transition Metal Phenylthiolates. The Isolation of the Perthiolate Salts [M(N-MeIm)₆](S₂Ph)₂

Ulrike Krautscheid, Somanath Dev, Harald Krautscheid, Partha P. Paul, Scott R. Wilson, Thomas B. Rauchfuss

Page range: 653-658

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Abstract

Salts of the composition [M(N-MeIm) 6 ](SPh) 2 (M = Mn, Ni; N-MeIm = N-methylimidazole) were prepared by dissolution of the metal powders with N-MeIm solutions of Ph 2 S 2 . X-ray crystallographic examination established that these salts indeed feature uncoordinated PhS - . The salts [M(N-McIm) 6 ](SPh) 2 (M = Mn, Ni) react with S 8 to give [M(N-MeIm) 6 ]S 8 via the intermediacy of the perthiolate salts [M(N-MeIm) 6 ](S 2 Ph) 2 .

Open Access June 2, 2014

Darstellung und Einkristall-Röntgenstrukturanalyse einiger Fluorphosphite und Phosphitester / Preparation and Single Crystal X-Ray Diffraction Study of Some Fluorophosphites and Phosphite Esters

Thomas G. Meyer, Axel Fischer, Peter G. Jones, Reinhard Schmutzler

Page range: 659-671

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Abstract

The synthesis of some monofluorophosphite esters from the appropriate hydroxy compound and PCl 2 F in the presence of a tertiary amine is described. The reaction of 2,2′-dihydroxy-biphenyl with PCl 3 in the presence of triethylamine did not furnish the expected chlorophosphite 9; instead, the bridged bisphosphite ester, 10, was obtained. Reaction of the fluorophosphite ester 8 with 3,5-di-tert-butyl-benzoquinone furnished the spiromonofluorophosphorane 12 in which λ 5 P is part of a five-membered and a seven-membered ring system. Single crystal X-ray diffraction studies were conducted on compounds 2, 10 and 13. In the case of 2, crystallographic 2/m symmetry and short intermolecular P · · · O distances were observed. Compound 10 shows short intramolecular P · · · O contacts. The catechyl phosphate 13, similarly to other dialkylphosphate esters, was found to be a hydrogen-bonded dimer.

Open Access June 2, 2014

Juglorubin

Holger Lessmann, Johann Krupa, Helmut Lackner, Karen Schmidt-Bäse, George M. Sheldrick

Page range: 672-682

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Abstract

The isolation of Juglorubin (2) from cultures of Streptomyces spp., which produce a series of other hydroxynaphthoquinones, is described. 2 is a unique, unusually condensed ionic colorant with the formula C 28 H 17 NaO 11 . The structure of 2 was elucidated by X-ray structure analysis of the acetyl dimethyl derivative 4. Detailled spectral information is given for the previously unknown benzindenylid-quinone molecule, e.g. the assignment of the 13 C NMR signals. 2 is probably formed in a complex reaction from two Juglomycin C units involving a late C—C-bond cleavage.

Open Access June 2, 2014

Notizen: Single-Crystal Structure Refinement of LiZnAs

Wolfgang Hönle

Page range: 683-684

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Abstract

The crystal structure of LiZnAs has been verified with single crystal X-ray methods. LiZnAs crystallizes in a filled-up zinc blende type of structure (F 43 m, a = 593.9(1) pm, As at site 4a (000); Zn at site 4d (3/4 3/4 3/4); Li at site 4 c (1/4 1/4 1/4); 25 hkl; R = 0.018). As is coordinated by 4 Li and 4 Zn atoms with identical distances of 257.2(1) pm. Li and Zn atoms are tetrahedrally coordinated by As. No indications for a disorder between Li and Zn have been found.

Open Access June 2, 2014

Notizen: The Crystal Structure of β-CsReO₄, the Room-Temperature Modification of Cesium Perrhenate

Peter Rögner, Klaus-Jürgen Range

Page range: 685-687

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Abstract

The crystal structure of β-CsReO 4 , the roomtemperature modification of cesium perrhenate, was determined from single-crystal X-ray data as orthorhombic, space group P nma, a = 5.7556(9), b = 5.9964(8), c = 14.310(2) Å and Z = 4. The structure was refined to R = 0.027, R w = 0.023 for 779 absorption-corrected reflections. It represents an orthorhombic distortion of the tetragonal high-temperature phase α-CsReO 4 . The structure of β-CsReO 4 comprises isolated ReO 4 tetrahedra, linked together by Cs ions. The average Re-O distance was found to be 1.714(4) Å.

Open Access June 2, 2014

Notizen: The Crystal Structure of Cesium Fluorotrioxosulfate(VI), CsSO₃F

Peter Rögner, Klaus-Jürgen Range

Page range: 688-690

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Abstract

The crystal structure of CsSO 3 F was determined from single-crystal X-ray data as tetragonal, space group I4,/amd, with a = 5.6317(2), c = 14.1991(9) Å and Z = 4. The structure was refined to R = 0.028,R w = 0.028 for 403 unique reflections. In contrast to the earlier literature CsSO 3 F is not isomorphous with scheelite but with α-CsReO 4 . The structure contains isolated SO 3 F tetrahedra which are linked together by twelvefold coordinated Cs ions. The average S–O,F distance is 1.453(3) Å.

Open Access June 2, 2014

Notizen: Preparation and Structure of Tris(acetylacetonato)silicon Dichloroargentate

Dietlinde Högerle, Ulrich Link, Ulf Thewalt

Page range: 691-693

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Abstract

The ionic compound [Si(acac) 3 ][AgCl2] · CH 2 C1 2 , (1) was synthesized by reaction of [Si(acac) 3 ][HCl 2 ] and silver acetate in dichloromethane. A singlecrystal X-ray analysis shows that the cation has an octahedral tris-chelate structure and that the anion is a polymeric chain, composed of edgesharing AgCl 4 tetrahedra.

Open Access June 2, 2014

Notizen: Über die Darstellung und spektroskopische Charakterisierung von CH₃S(Br)F⁺SbF₆^- / On the Preparation and Spectroscopic Characterization of CH₃S(Br)F⁺SbF₆-

Rolf Minkwitz, Birgit Bäck

Page range: 694-696

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Abstract

CH 3 S(H) + SbF 6 - reacts in HF as solvent with Br 2 to form CH 3 S(Br)F + SbF 6 - . The salt is stable below 195 K and has been characterized by vibrational and 1 H and 19 F NMR spectroscopy.

About this journal

Objective
Zeitschrift fuer Naturforschung B (ZNB) publishes novel research in all areas of inorganic chemistry, organic chemistry, and analytical chemistry. In particular, the journal focuses on solid state chemistry, coordination chemistry, main group element chemistry, synthetic organic chemistry, natural product chemistry and, to a lesser extent, on analytical chemistry. For more than 65 years Zeitschrift fuer Naturforschung B has been open to contributions from all fields of experimental and theoretical chemistry. Zeitschrift fuer Naturforschung B publishes 12 issues per volume/year. Sometimes double issues occur.

Topics

Solid state chemistry
Coordination chemistry
Main group element chemistry
Organic chemistry
Natural product chemistry

Article formats
Original (full) papers, research notes and preliminary communications, reports on specific research topics of current interest (reviews)

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Volume 48 Issue 5

Issue of Zeitschrift für Naturforschung B

Na2TiOS2 — Ein Oxothiotitanat(IV) mit unendlichen Tetraederketten / Na2TiOS2 — An Oxothiotitanate(IV) with Infinite Tetrahedral Chains

Abstract

Clusterdithiophosphinate mit kubanartigem Mo2M2S4-Kern (M = Co, W) / Clusterdithiophosphinates with Cubane-Type Mo2M2S4-Core (M = Co, W)

Abstract

X-Ray Structural Analysis and Vibrational Spectra of Sodium Cysteine-S-sulfonate, +H3NCH(COO-)CH2S2O3Na • 3/2H2O [1]

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Reaktionen von Pyridin-Basen mit Na/K-Legierung und Diorganylaminodifluorboranen / Reactions of Pyridine-Bases with Na/K-Alloy and Diorganylaminodifluoroboranes

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Addukte Aromat/Chlorwasserstoff bei tiefen Temperaturen: Beiträge zu Bildung und Kristallstruktur [1] / Adducts Arene/Hydrogen Chloride at Low Temperatures: Contributions to Formation and Crystal Structure [1]

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Oligophosphan-Liganden, XXXVIII / Oligophosphine Ligands, XXXVIII

Darstellung, Isomerie und Reaktivität von Arylhydridoruthenium(II)-Komplexen [MeSi(CH2PMe2)3l(Me3P)RuH(Ar) / Preparation, Isomerism, and Reactivity of Arylhydridoruthenium(II) Complexes [MeSi(CH2PMe2)3](Me3P)RuH(Ar)

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Syntheses and Structures of Three Mononuclear Coordination Compounds Containing Six- and Seven-Coordinated Manganese(II) Ions

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Titan(IV)-Fulvalenkomplexe. Darstellung und Struktur von [CpTiPh2l2(C10H8) / Titanium(IV) Fulvalene Complexes. Preparation and Structure of [CpTiPh2]2(C10H8)

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Bis(di-tert-butylphosphino)ethan-nickel(0)-Komplexe / Bis(di-tert-butylphosphino)ethane-nickel(0) Complexes

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Darstellung und Eigenschaften von CH3C(CH2PPh2)3MoCl3 / Characterization and Properties of CH3C(CH2PPh2)3MoCl3

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N-Methylimidazole Mediated Chemistry of Transition Metal Phenylthiolates. The Isolation of the Perthiolate Salts [M(N-MeIm)6](S2Ph)2

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Darstellung und Einkristall-Röntgenstrukturanalyse einiger Fluorphosphite und Phosphitester / Preparation and Single Crystal X-Ray Diffraction Study of Some Fluorophosphites and Phosphite Esters

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Juglorubin

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Notizen: Single-Crystal Structure Refinement of LiZnAs

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Notizen: The Crystal Structure of β-CsReO4, the Room-Temperature Modification of Cesium Perrhenate

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Notizen: The Crystal Structure of Cesium Fluorotrioxosulfate(VI), CsSO3F

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Notizen: Preparation and Structure of Tris(acetylacetonato)silicon Dichloroargentate

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Notizen: Über die Darstellung und spektroskopische Charakterisierung von CH3S(Br)F+SbF6- / On the Preparation and Spectroscopic Characterization of CH3S(Br)F+SbF6-

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Na₂TiOS₂ — Ein Oxothiotitanat(IV) mit unendlichen Tetraederketten / Na₂TiOS₂ — An Oxothiotitanate(IV) with Infinite Tetrahedral Chains

Clusterdithiophosphinate mit kubanartigem Mo₂M₂S₄-Kern (M = Co, W) / Clusterdithiophosphinates with Cubane-Type Mo₂M₂S₄-Core (M = Co, W)

X-Ray Structural Analysis and Vibrational Spectra of Sodium Cysteine-S-sulfonate, ⁺H₃NCH(COO-)CH₂S₂O₃Na • 3/2H₂O [1]

Darstellung, Isomerie und Reaktivität von Arylhydridoruthenium(II)-Komplexen [MeSi(CH₂PMe₂)₃l(Me₃P)RuH(Ar) / Preparation, Isomerism, and Reactivity of Arylhydridoruthenium(II) Complexes [MeSi(CH₂PMe₂)₃](Me₃P)RuH(Ar)

Titan(IV)-Fulvalenkomplexe. Darstellung und Struktur von [CpTiPh₂l₂(C₁₀H₈) / Titanium(IV) Fulvalene Complexes. Preparation and Structure of [CpTiPh₂]₂(C₁₀H₈)

Darstellung und Eigenschaften von CH₃C(CH₂PPh₂)₃MoCl3 / Characterization and Properties of CH₃C(CH₂PPh₂)₃MoCl3

N-Methylimidazole Mediated Chemistry of Transition Metal Phenylthiolates. The Isolation of the Perthiolate Salts [M(N-MeIm)₆](S₂Ph)₂

Notizen: The Crystal Structure of β-CsReO₄, the Room-Temperature Modification of Cesium Perrhenate

Notizen: The Crystal Structure of Cesium Fluorotrioxosulfate(VI), CsSO₃F

Notizen: Über die Darstellung und spektroskopische Charakterisierung von CH₃S(Br)F⁺SbF₆^- / On the Preparation and Spectroscopic Characterization of CH₃S(Br)F⁺SbF₆-