Published by De Gruyter

Volume 43 Issue 8

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Di(μ-phosphido)cobalt-und -nickel-Verbindungen mit Trimethylphosphanliganden/ Di(μ-phosphido)cobalt and Nickel Compounds with Trimethylphosphine Ligands

Hans-Friedrich Klein, Michael Gaß, Ulf Zucha, Brigitte Eisenmann

Page range: 927-932

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Abstract

Several fortuitous preparations and high yield rational syntheses for [(Me 3 P) 2 M(PMe 2 )]: (1: M = Co; 2: M = Ni) are described. 1 crystallizes in the space group P1̄ (no. 2); a = 975.6(5). b = 943.6(5), c - 904.2(5) pm. α= 63.8(1)°, β = 79.1(1)°, γ = 72.8(1)°. Mixed metal complexes L 2 Co(PR 2 ) 2 NiL 2 (L = PMe 3 ; R = Me, Ph) evaded detection giving symmetric products exclusively. An improved synthesis of LiP(C 6 H 5 ) 2 ·dioxane is also described.

Open Access June 2, 2014

N,N′-Bis(diphenyIphosphino)-S,S-dimethylsulfodiimin – ein Ligand für cyclische Übergangsmetallkomplexe/ N,N′-Bis(diphenylphosphino)-S,S-dimethylsulfodiimine – a Ligand for Cyclic Transition Metal Complexes

Herbert W. Roesky, Michael Zimmer, Regine Herbst, George M. Sheldrick

Page range: 933-936

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Abstract

Me 2 SN 2 P 2 Ph 4 M(CO) 4 complexes (1) (M: 1 a Cr, 1 b Mo, 1 c W) have been synthesized from Me 2 S(NPPh 2 ) 2 and C 7 H 8 M(CO) 4 . 1a-1c are stable at room temperature, 1 b crystallizes in the space group P2 1 2 1 2 with cell constants a = 2486.3(2); b = 1488.8(1); c = 882.0(1) pm.

Open Access June 2, 2014

Synthese und Struktur eines ungewöhnlichen Molybdän-Heterocyclus durch Substitution eines Phenylringes in ortho-Stellung/ Synthesis and Structure of an Unusual Molybdenum Heterocycle by Substitution of a Phenyl Ring in ortho-Position

Uwe Scholz, Mathias Noltemeyer, Herbert W. Roesky

Page range: 937-940

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Abstract

The new ligand (Me 3 Si) 2 NC(Ph)NP(Ph) 2 N(SiMe 3 ) (1) reacts with MOOCl 4 to yield the green metallacycle 4. 4 was characterized by X-ray diffraction. Crystals of 4 are monoclinic, space group P2 1 /n with a = 1061.2(10). b = 1590.5(10), c = 1737.4(20) pm, β = 104.84(7)° and Z = 4. Mo is coordinated octahedrally by two nitrogens of the bifunctional ligand. by one oxygen and three chlorine atoms. The ligand undergoes cyclization, a bond being formed between N and one phenylic o-position.

Open Access June 2, 2014

Reaktionen der höheren Halogenide des Niobs, Molybdäns und Wolframs mit dem Phosphor-Ylid (Et₂N)₃P=CH₂ - Röntgenstruktur von [(Et₂N)₃PCH₂]₂²⁺[WCl₆]^2-/ Reactions of the Higher Halides of Niobium, Molybdenum and Tungsten with the Phosphorus-Ylid (Et₂N)₃P=CH₂– X-Ray Structure of [(Et₂N)₃PCH₂]₂²⁺[WCl₆]^2-

Herbert W. Roesky, Bernhard Mainz, Mathias Noltemeyer, George M. Sheldrick

Page range: 941-944

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Abstract

(Et 2 N) 3 P=CH 2 reacts with NbCl 5 , WCl 6 or WF 6 under C-C bond formation to give the phosphonium cation [(Et 2 N) 3 PCH 2 ] 2 2+ · [(Et 2 N) 3 PCH 2 ] 2 2+ [WCl 6 ] 2 - was isolated in a crystalline form and investigated by X-ray analysis. The reaction of (Et 2 N) 3 P=CH 2 with MOCl 4 in a solvent proceeds with formation of the [(Et 2 N) 3 PCH ] + cation.

Open Access June 2, 2014

[Fe(CO)₄C(O)NMe₂][C(NMe₂)₃]; die erste Strukturbestimmung einer Organometallverbindung mit dem Carbeniumion [C(NMe₂)₃]⁺/ [Fe(CO)₄C(O)NMe₂][C(NMe₂)₃]; the First Structure Determination on an Organometallic Compound with the Carbenium Ion [C(NMe₂)₃]⁺

Roland Boese, Dieter Bläser, Wolfgang Petz

Page range: 945-948

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Abstract

The crystal structure of the carbamoyl complex [(CO) 4 FeC(O)NMe 2 ][C(NMe 2 ) 3 ] (1) is described. It crystallizes in the triclinic space group PI (a = 7.876(3), b = 10.098(3), c = 12.067(5)Å, α = 94.25(3), β = 90.94(3), γ = 97.30(3)°, Z = 2) and consists of independent ions. The cation has a planar CN 3 array with sp 2 hybridized C and N atoms. The carbamoyl group of the anion occupies an axial position in the trigonal bipyramidal environment of the iron atom.

Open Access June 2, 2014

Über die Reaktion von Dicyan mit Cd(II)-Ionen Röntgenstrukturanalyse von [Cd{(CN)₂}₂SO₂ ][AsF₆]₂/ The Reaction of Cyanogen with Cd(II) Ions X-Ray Structure Analysis of [Cd{(CN)₂}₂SO₂][AsF₆]₂

Herbert W. Roesky, Jürgen Schimkowiak, Mathias Noltemeyer, George M. Sheldrick

Page range: 949-951

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Abstract

Cd[AsF 6 ] 2 (1) reacts with cyanogen to yield [Cd{(CN) 2 } 2 SO 2 ][AsF 6 ] 2 (2). 2 crystallizes in the space group Pnma with cell constants a = 1475.2(3); b = 821.7(3); c = 1321.2(9) pm. The coordination sphere of cadmium consists of nine atoms (one oxygen, four fluorines and four nitrogens). Cyanogen forms polymeric links.

Open Access June 2, 2014

Element–Element-Bindungen, IV. Molekül-und Kristallstruktur des Tetramethyldiphosphans und -diarsans /Element–Element Bonds, IV. Molecular and Crystal Structure of Tetramethyldiphosphane and -diarsane

Otto Mündt, Heinz Riffel, Gerd Becker, Arndt Simon

Page range: 952-958

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Abstract

The molecular and crystal structures of the isotypic compounds tetramethyldiphosphane 1 and -diarsane 2 have been determined by single crystal X-ray diffraction (monoclinic; C2/m; Z = 2; 1/2: -155/-144 °C\a = 540.6(2)/555.8(2); b = 1131.0(6)/l 136.7(6); c -602.5(2)/612.8(2) pm;β = 97.31(3)/95.24(3)°;P-P 221.2(1)/As-As 242.9(1) pm). In accordance with the crystallographically imposed symmetry 2/m, the molecules adopt antiperiplanar conformation. Their crystal structures are closely related to those of the homologues tetramethyldistibane 3 [1] and -dibismuthane 4 [3]. As found for the latter compounds, the E -E units (E = P, As) are also aligned in linear chains, but the intermolecular E···E contacts (P···P 381/As···As 370 pm) do not allow any extended interaction between molecules, which otherwise would result in thermochromic effects.

Open Access June 2, 2014

Untersuchungen zur Ringkontraktion am 1,4-Dithia-2,6-diaza-3,5-diborinan-System/ Studies on Ring Contraction of the l,4-Dithia-2,6-diaza-3,5-diborinane System

Carl Habben, Anton Meiler, Stefan Pusch

Page range: 959-962

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Abstract

The 1,4-dithia-2,6-diaza-3,5-diborinanes 1a-d react with elemental sodium with formation of the 1,3-diaza-2,4-diboretidines 2a-d. By use of more sodium in case of 1 d or 3,5-bis(diethylamino)- 2-cyclohexyl-6-trimethylsilyldiborinane, the 1,3-thiaza-2,4-diboretidines 3 were formed. 3.5-Dimethyl-2,6-bis(trimethylsilyl)-1,4-dithia-2,6-diaza-3,5-diborinane gives the borazine 4, The reaction of di-t-butyl-sulfurdiimide with 2,6-di-t-butyl-3,5-dimethyl-1,4-dithia-2,6-diaza-3,5-diborinane leads by ring contraction to the four-membered ring system 5. 1 H, 11 B, 13 C NMR and mass spectra are reported and discussed.

Open Access June 2, 2014

Aluminiumbromid-Pyridiniumbromid-Verbindung: Kristallstruktur Kristallstrukturbestimmung von [Tris(pyridinium)bromid]bis(tetrabromoaluminat(III))/ Aluminiumbromide-Pyridiniumbromide Compounds: Crystal Structure Crystal Structure Determination of [Tris(pyridinium)bromide]bis(tetrabromoaluminate(III))

Harald Burger, Karl Hensen, Peter Pickel

Page range: 963-965

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Abstract

The compound [(PyH) 3 Br][AlBr 4 ] 2 is formed by melting stoichiometric amounts of AlBr/PyHBr in a ratio of 2:3. It crystallizes in the orthorhombic space group Pbca with lattice constants a = 1365.5(2), b = 1616.0(2), c = 2783.7(3) pm, Z = 8, D c = 2.21 g/cm 3 . The structure was solved from 2810 diffractometer measured intensities (Cu -K α radiation) and refined to R w (F) = 0.071. The cation shows three pyridinium ions attached via N - H - Br hydrogen bonds to a central bromide ion. The N - Br distances are 321(1), 321(2) and 332(2) pm.

Open Access June 2, 2014

Polymorphie von Tellur(IV)-iodid/ Polymorphism of Tellurium(IV) Iodide

Rüdiger Kniep, Heinz Jürgen Beister, Dieter Wald

Page range: 966-980

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Abstract

Idiomorphous crystals of five different polymorphic modifications (α-ε) of TeI 4 are simultaneously grown from solutions of TeI 4 and concentrated HI in methanol by evaporating the solvent at room temperature. δ-TeI 4 is the only stable phase at normal conditions. Phase transformations of α-, β-, γ-and ε-TeI 4 to the final stage δ-TeI 4 take place by heating and run through discrete intermediates. The observed graduations lead to a sequence γ-, β-, α-,ε-TeI 4 which indicates “increasing metastability”. The crystal structures of α-TeI 4 (trigonal; P3̄ml; a = 4.228(2), c - 6.684(6)Å, Z = 0.5; D x = 5.10 g/cm 3 ), β-TeI 4 (orthorhombic; Pn2 1 m; a = 6.888(2), b = 14.539(3), c = 16.753(4) Å, Z = 8; D x = 5.03 g/cm 3 ) and γ-TeI 4 (monoclinic; P2 1 /c; a = 11.199(4), b = 13.599(4), c = 22.158(6) Å,β = 98.10(3)°, Z = 16; D, = 5.05 g/cm 3 ) are related to the known crystal structure of δ-TeI 4 . α-TeI 4 (“Te 0.5 I 2 ”) is an isotype of the 2H-CdI : structure with random distribution of Te over the Cd-positions. The crystal structures of β-, γ-and δ-TeI 4 contain discrete tetrameric molecules “(TeI 4 ) 2 (TeI 3 + I - ) 2 ” which are generated by ordered distributions of Te over 1/4 of the octahedral holes of a 2H-(β) and a 4H-sequence (y,δ ) of the nearly close packed iodine layers. A nearly cubic close packing of Iodine atoms is observed in the crystal structure of ε-TeI 4 (tetragonal; I4 1 /amd; a = 16.875(6), c -11.829(5) Å, Z = 16; D x = 5.01 g/cm 3 ). The ordered distribution of Te in 1/4 of the octahedral holes leads to tetrameric molecules “(TeI 3 + I - ) 4 ” in a cubanelike arrangement which, thus far, has been observed only in the crystal structures of TeCl 4 and TeBr 4 . The Madelung Parts of Lattice Energies, MAPLE, of β-, γ-, δ-and ε-TeI 4 are calculated.

Open Access June 2, 2014

Synthese, Eigenschaften und Kristallstruktur von (NH₄)NbOBr₄/ Synthesis, Properties and Crystal Structure of (NH₄)NbOBr₄

Manfredo Hörner, Wolfgang Hiller, Joachim Strähle, George M. Sheldrick

Page range: 981-984

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Abstract

(NH 4 )NbOBr 4 is obtained as air sensitive, light red crystals from NH 4 Br and NbBr 5 in a sealed glass ampoule at 420 °C, whereby the oxygen presumably originates from the glass surface. The compound crystallizes in the monoclinic space group C2/m with a = 1269.9(1), b = 1384.7(2). c = 773.0(2) pm, β = 114.44(2)° and Z = 6. The structure is built up by NH 4+ cations and polymeric NbOBr 4 anions. Symmetrical linear oxo bridges with Nb-O = 199 pm connect square planar NbBr 4 units to form endless chains arranged in planes parallel (010). Neighbouring NbBr 4 units are in eclipsed as well as staggered orientations. The NH 4 + cations are located between the planes of parallel NbOBr 4 - chains. The vibrational frequencies of the IR and Raman spectrum are assigned.

Open Access June 2, 2014

Unsymmetrisch substituierte Phosphinoschwefeldiimide – NMR-Untersuchungen über die Konfiguration in Lösung/ Unsymmetrically Substituted Phosphino Sulfur Diimides – NMR Studies on the Configuration in Solution

Max Herberhold, Stefan M. Frank, Bernd Wrackmeyer

Page range: 985-992

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Abstract

The phosphino-substituted sulfur diimides S(N-P t Bu 2 ) 2 (1), t Bu;P(NSN)PRR′ (R = R′ - phenyl (2a), cyclohexyl (2b), isopropyl (2c), ethyl (2d); R = phenyl, R′ = tert-butyl (2e)) and t Bu 2 P(NSN) t Bu (3) were studied in solution by 1 H, 13 C and 31 P NMR spectroscopy**. The coupling constants 4 J( 31 P 31 P) of the compounds containing different phosphino groups, 2a-e, depend both on the nature of the solvent and the temperature. The NMR results are interpreted in accord with a rapid Z/E⇄ E/Z interconversion at room temperature and the predominance of a single configurational isomer at low temperatures. There is no indication for the presence of the “symmetrical” configurations, Z/Z or E/E respectively, in solution in appreciable amounts. 15 N NMR data are also reported for a series of sulfur diimides.

Open Access June 2, 2014

Komplexe mit aromatischen Carbonsäuren, IV. Ca₂[C₆H₂(COO)₄]·6H₂O - Eine neue Schichtstruktur/ Complexes with Aromatic Carboxylic Acids, IV. Ca₂[C₆H₂(COO)₄]·6H₂O - A Novel Layer Structure

Christian Robl

Page range: 993-997

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Abstract

Single crystals of Ca 2 [C 6 H 2 (COO) 4 ]·6H 2 O were grown in aqueous silica gel. Ca 2+ has CN 6+2. The coordination polyhedron is formed by three water molecules and five oxygen atoms of carboxylate groups. Six oxygen atoms are closely bound (235,9-243,9 pm), the two remaining coordination partners are considerably more remote from Ca 2+ (268,2 and 273,8 pm). COO - groups chelate Ca 2+ in an asymmetric manner, but the C -O bond lengths do not differ markedly (125,2-126,3 pm). The connection of Ca 2+ with [C 6 H 2 (COO) 4 ] 4- leads to rigid layers. Adjacent layers are interlinked by hydrogen bonds. Those oxygen atoms which are weakly bound to Ca 2+ are favoured as proton acceptors in hydrogen bonds. The COO groups are tilted differently against the C 6 -ring plane. One is approximately coplanar, but the other is oriented almost perpendicularly.

Open Access June 2, 2014

Darstellung von Dichalkogenostibanen des Typs RSb(ER′)₂ (R = CH₃, C₂H₅; E = S, Se; R = CH₃, C₆H₅)/ Preparation of Dichalcogenostibanes of the Type RSb(ER′)₂ (R = CH₃, C₂H₅; E = S, Se; R′ = CH₃, C₆H₅ )

Hans Joachim Breunig, Sabahittin Güleç

Page range: 998-1002

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Abstract

Dichalcogenostibanes of the type RSb(ER′) 2 (R = CH 3 ,C 2 H 5 ; E = S. Se; R′ = CH 3 . C 6 H 5 ) and trialkylstibanes R 3 Sb have been prepared by redistribution reactions of stibanes of the type R 2 SbER′.

Open Access June 2, 2014

Zur Stereochemie des freien Elektronenpaares in AX6E-Systemen, VIII. Statisch verzerrte Anionen in [H₃N(CH₂)₃NH₃]₃(BiX₆)₂(H₂O)₂ mit X = Cl, Br/ On the Stereochemistry of the Lone-Pair Electrons in AX₆E-Systems, VIII Statically Distorted Anion in [H₃N(CH₂)₃NH₃]₃(BiX₆)₂(H₂O)₂ with X = Cl, Br

André du Bois, Walter Abriel

Page range: 1003-1009

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Abstract

Using 293 K diffractometer intensity data, the crystal structures of [H 3 N(CH 2 ) 3 NH 3 ] 3 (BiX 6 ) 2 (H 2 O) 2 with X - Cl, Br have been determined by single crystal X-ray technique and refined to a final R w of 0.027 and 0.043, respectively. The structures are isotypic, space group P2 1 /c, Z = 2 with a = 14.415(1). b = 9.7401(7), c = 12.4609(9)Å, β = 105.997(8)°for X - Cl and a = 14.794(2), b = 10.127(2), c = 12.853(2)Å, β = 105.68(2)° for X - Br. Statically distorted BiX 6 3- octahedra confirm the symmetry rules for the stereochemistry of the lone pair electrons in AX 6 E-systems. Basic structural data for all compounds containing BiX 6 3- and SbXh 3 ions (X = Cl, Br, I) known to date are given including the ⊿-values as a measure for the distortion of the octahedral coordination polyhedron.

Open Access June 2, 2014

Triazaphosphinine – Reaktionen, Zwitterionen, P–B-Austausch/ Triazaphosphinines – Reactions, Zwitter Ions, P – B-Exchange

Matthias Meyer, Johannes Kadel, Heinz Oberhammer

Page range: 1010-1016

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Abstract

2,2-Dichloro-triazaphosphinine (2) reacts with SbF 3 in the molar ratio 3:1 to give the mixed halogenated triazaphosphinine (3). New addition compounds 5 and 6 can be formed in the reaction of the zwitter ion 4 and amines or in the reaction of 2.2-difluoro-triazaphosphinine (1) with KCN. Phosphorus-boron-exchange is observed in the reactions of 4 or 2 with BF 3 · OEt 2 . The new C-B -N-heterocycles 8 and 9 are obtained. The gas-phase structure of 1 has been determined by electron diffraction. The scattering intensities are compatible with a planar ring conformation with C 2v symmetry and with equivalent NC bond lengths (PN = 1.579(10) Å, NC = 1.299(7) Å, NPN = 109.2(7)°, PNC - 118.1(9)°, CNC - 119.6(7)° and NCN = 127.5(12)°).

Open Access June 2, 2014

NaGaSn₅, eine neue Zintl-Phase mit Ga–Sn-Schrauben/ NaGaSn5, a New Zintl Phase Containing Ga–Sn Helices

Wolfgang Blase, Gerhard Cordier

Page range: 1017-1019

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Abstract

NaGaSn, (trigonal; P3 1 12 (No. 151); a = 632.8(4), c = 617.0(3) pm, Z - 1; d x = 5.33 g/cm 3 ) was grown from the melt. The crystal structure contains Ga and Sn atoms in a helical arrangement (six atoms per turn) along the c-axis direction. Interatomic bonding between neighbouring helices completes a distorted [2+2]-tetrahedral environment for every Ga/Sn position. The compound is classified in terms of the Zintl concept.

Open Access June 2, 2014

Synthese und Eigenschaften von tert-Butyltriiodsilan/ Synthesis and Properties of tert-Butyltriiodosilane

Marianne Baudler, Uwe Arndt, Detlef Grenz

Page range: 1020-1022

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Abstract

tert-Butyltriiodosilane (1) has been prepared in its pure form by heating tert-butylsilane (2) with iodine. Compound 1 has been characterized by elemental analysis as well as by spectroscopic methods.

Open Access June 2, 2014

Zur Polymorphie von TbCI₃/ Polymorphism of TbCl₃

Harald Gunsilius, Horst Borrmann, Arndt Simon, Werner Urland

Page range: 1023-1028

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Abstract

3 different modifications of TbCl 3 were synthesized. TbCl, (UCl 3 -type), probably in a metastable state, crystallizes in space group P6 3 /m with a = 737.63(2) pm, c = 405.71(2) pm and Z - 2. TbCl 3 (PuB 3 -type) crystallizes in space group Cmcm with a = 384.71(6) pm, b = 1177.37(7) pm. c = 851.77(4) pm and Z = 4. h-TbCl 3 , the high temperature phase being stable above 790 K. crystallizes in space group P4 2 /mnm with a = 642.51(4) pm, c = 1177.14(18) pm and Z = 4.

Open Access June 2, 2014

Synthese und Kristallstruktur von (Cyclopentadienyl)(dicarbonyl)(1,5-di-/Molyl-pentaazadienido)molybdän, (Cp)Mo(CO)₂(tolN₅tol)/ Synthesis and Crystal Structure of (Cyclopentadienyl)(dicarbonyl)(1,5-di-p-tolyl-pentaazadienido)molybdenum, (Cp)Mo(CO)₂(tolN₅tol)

Johannes Beck

Page range: 1029-1032

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Abstract

(Cp)Mo(CO) 2 (tolN 5 tol) is formed in the reaction of (Cp)Mo(CO) 3 Cl with tolNN(NH)NNtol and NaOH in ethanol. It forms red platelike crystals from THF/hexane which crystallize in the monoclinic space group P2 1 /n with the lattice parameters a = 765.6(2), b = 2372.3(3), c = 1149.4(2) pm, β = 97.06(2)°, Z = 4. The structure consists of monomeric complexes. The pentaazadienido ligand chelates with its nitrogen atoms N1 and N3 the Mo atom of a (Cp)Mo(CO) 2 unit. The nitrogen atom N 5 is not coordinated to the metal atom. Although asymmetrically bonded, the all trans N 5 zig zag chain is planar. The N -N distances in the four membered chelate ring are nearly equal (N 1 - N 2 = 131.0 and N 2 - N 3 = 132.6 pm)

Open Access June 2, 2014

[Fe(phen)₃]₂Sb₆l₂₂·2CH₃CN: Ein Iodoantimonat mit zentralem [Sb₆I₆]-Doppelwürfel (phen = 1,10-Phenanthrolin)/ [Fe(phen)₃]₂Sb₆I₂₂ · 2 CH₃CN: An Iodoantimonate with Central [Sb₆I₆]-Double Cube (phen = 1,10-Phenanthrolin)

Siegfried Pohl, Detlev Haase, Rainer Lötz, Wolfgang Saak

Page range: 1033-1037

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Abstract

Reaction of [Fe(phen) 3 ]I 2 (phen = 1.10-Phenanthrolin) with Sbl 3 in acetonitrile leads to [Fe(phen) 3 ] 2 Sb 6 I 22 ·2CH 3 CN (1). The structure of 1 was determined from single crystal X-ray diffraction data. 1 crystallizes in the triclinic space group P1̄ with a = 1352.4(1). b - 1376.8(1), c - 1597.7(1) pm, α = 105.85(1). β = 92.09(1). γ = 97.94(1)°. Z = 1. The structure of 1 consists of isolated anions and cations. The centrosymmetric Sb 6 I 22 4- ion exhibits a double cube-like structure with Sb and I occupying alternating corners of the skeleton.

Open Access June 2, 2014

Synthesis and Activity of Juvenile Hormone Analogues (JHA)

Juan B. Rodriguez, Eduardo G. Gros, Angel M. Stoka

Page range: 1038-1042

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Abstract

From geranylacetone and by the use of a variety of reagents, twelve analogues of the juvenile hormone III were synthesized. The compounds (5-16) have an isoprenic structure bearing at the extreme of the chain functional groups as carbonate, carbamate, thiolcarbonate, thiolcarbamate, carbonyloxyimino and thiol carbonyloxyimino. Compounds 5-9 present the normal unsaturated isoprenic chain while compounds 10-16 have a monoepoxide function. All the compounds were tested for their respective juvenile hormone activity for Triatoma infestans and Rhodniusprolixus. The most active compounds were those having a thiol carbonate group independently of the oxidation state of the molecule. The synthetic procedures and the biological results are discussed.

Open Access June 2, 2014

meso-Substituierte Porphyrine, 5. Korbporphyrine meso-Substituted Porphyrins, 5. Basket Porphyrins

Heinrich Volz, Michael Hassler

Page range: 1043-1052

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Abstract

2-Pyrryl-(m-terphenyl)-carbinol and 2-pyrryl-(3,3″,5.5″-tetra-t-butyl-m-terphenyl)-carbinol are cyclized in acidic medium to the corresponding raeso-tetraarylporphyrins. The meso-tetraarylporphyrins are transferred to the iron and manganese complexes. The reactions of the iron porphyrins with OH - are studied and the products of these reactions are characterized.

Open Access June 2, 2014

The Crystal Structure of Potassium Nickel Arsenate; KNiAsO₄

A. M. Buckley, S. T. Bramwell, P. Day, W. T. A. Harrison

Page range: 1053-1055

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Abstract

The crystal structure of potassium nickel arsenate. KNiAsO 4 has been determined by high resolution powder neutron diffraction at 30 K. The unit cell of KNiAsO 4 is rhombohedral. space group R3̄, with hexagonal cell constants, a = 4.97208(2) (Å). c = 28.52606(10) (Å). The compound is isomorphous with NaNiAsO 4 .

Open Access June 2, 2014

Nicotinamide Nucleotides in Different Types of Human Cataractous Lenses

Tanweer Sarwat, M. Ataur Rahman, T. H. Kirmani

Page range: 1056-1058

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Abstract

The ratios of reduced and oxidized nicotinamide nucleotides (NADH/NAD + and NADPH/ NADP + ) were indirectly determined at various stages of cataractogenesis by estimating the concentrations of metabolites (lactate, pyruvate and malate) of the lens. The ratios of NADH/NAD + and NADPH/NADP + decreased significantly from immature to mature (P<.001, P<.05). to hypermature (P<.001, P<.05), to Morgagnian (Pc.001. Pc.001) and diabetic types (Pc.001, P < .001) of cataractous lenses respectively. Ratios of nicotinamide nucleotides in diabetic lenses were lower in comparison to those of other types studied. As the opacity progressed, the ratios decreased with increase in blood glucose levels.

Open Access June 2, 2014

The Structure and Absolute Configuration of Cyclotirucanenol, a New Triterpene from Euphorbia tirucalli Linn

Abdul Qasim Khan, Zaheer Ahmed, Najam-ul-Hussain Kazmi, Abdul Malik, Nighat Afza

Page range: 1059-1062

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Abstract

The structure and absolute configuration of “cyclotirucanenol” a new triterpene isolated from Euphorbia tirucalli has been established as 24β-methyl-9β-19-cyclolanost-20-en-3β-ol through chemical and spectroscopic studies including 2D-NMR.

Open Access June 2, 2014

Ceramid-1-phosphoethanolamine aus Myxococcus stipitatus/ Ceramide-1-phosphoethanolamines from Myxococcus stipitatus

J. Stein, H. Budzikiewicz

Page range: 1063-1068

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Abstract

The structures of six ceramide-1-phosphoethanolamines have been elucidated which differ in the long chain base as well as in the fatty acid component

Open Access June 2, 2014

Notizen: Synthese und Kristallstruktur von PPh₃Me[HSO₄]/ Synthesis and Crystal Structure of PPh₃Me[HSO₄]

Fritjof Schmock, Aida Müller, Ulrich Müller, Kurt Dehnicke

Page range: 1069-1071

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Abstract

PPh 3 Me[HSO 4 ] was prepared by the reaction of (PPh 3 Me)I with silver sulfate in aqueous solution. OPPh 2 Me and benzene being the by-products. The title compound was characterized by its IR spectrum as well as by an X-ray structure determination (1730 observed independent reflexions, R = 0.043). Crystal data: a = 910.4(3). b = 1587.8(4), c = 1294.2(6) pm, β = 105.52(3)°. space group P2 1 /c, Z = 4. The structure consists of PPh3Me ⊕ cations and of HOSO 3 ⊖ ions that are associated via strong hydrogen bonds to dimeric centrosymmetric units.

Open Access June 2, 2014

Notizen: High-field (500 MHz) ¹H NMR Spectra of Retinoic Acids and Arotinoids by Two-dimensional Chemical Shift Correlation (2D) Spectroscopy

Bruno Perly, Giuseppe C. Pappalardo, Michael Klaus, Enzo Montoneri

Page range: 1072-1074

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Abstract

The 1 H NMR spectra (in DMSO solution at 300 K) of retinoic acids (cis- and trans-isomers) and new arotinoids were run at 500 MHz and assigned by using homo- and heteronuclear two-dimensional (2D) chemical shift correlation experiments. Spectral analysis was indicating, on the basis of 7 values, that the ring C(l)-C(2)-C(3)-C(4)-C(5)-C(6) adopts, in all compounds, a chair conformation.

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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

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

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Volume 43 Issue 8

Issue of Zeitschrift für Naturforschung B

Di(μ-phosphido)cobalt-und -nickel-Verbindungen mit Trimethylphosphanliganden/ Di(μ-phosphido)cobalt and Nickel Compounds with Trimethylphosphine Ligands

Abstract

N,N′-Bis(diphenyIphosphino)-S,S-dimethylsulfodiimin – ein Ligand für cyclische Übergangsmetallkomplexe/ N,N′-Bis(diphenylphosphino)-S,S-dimethylsulfodiimine – a Ligand for Cyclic Transition Metal Complexes

Abstract

Synthese und Struktur eines ungewöhnlichen Molybdän-Heterocyclus durch Substitution eines Phenylringes in ortho-Stellung/ Synthesis and Structure of an Unusual Molybdenum Heterocycle by Substitution of a Phenyl Ring in ortho-Position

Abstract

Abstract

[Fe(CO)4C(O)NMe2][C(NMe2)3]; die erste Strukturbestimmung einer Organometallverbindung mit dem Carbeniumion [C(NMe2)3]+/ [Fe(CO)4C(O)NMe2][C(NMe2)3]; the First Structure Determination on an Organometallic Compound with the Carbenium Ion [C(NMe2)3]+

Abstract

Über die Reaktion von Dicyan mit Cd(II)-Ionen Röntgenstrukturanalyse von [Cd{(CN)2}2SO2 ][AsF6]2/ The Reaction of Cyanogen with Cd(II) Ions X-Ray Structure Analysis of [Cd{(CN)2}2SO2][AsF6]2

Abstract

Element–Element-Bindungen, IV. Molekül-und Kristallstruktur des Tetramethyldiphosphans und -diarsans /Element–Element Bonds, IV. Molecular and Crystal Structure of Tetramethyldiphosphane and -diarsane

Abstract

Untersuchungen zur Ringkontraktion am 1,4-Dithia-2,6-diaza-3,5-diborinan-System/ Studies on Ring Contraction of the l,4-Dithia-2,6-diaza-3,5-diborinane System

Abstract

Abstract

Polymorphie von Tellur(IV)-iodid/ Polymorphism of Tellurium(IV) Iodide

Abstract

Synthese, Eigenschaften und Kristallstruktur von (NH4)NbOBr4/ Synthesis, Properties and Crystal Structure of (NH4)NbOBr4

Abstract

Unsymmetrisch substituierte Phosphinoschwefeldiimide – NMR-Untersuchungen über die Konfiguration in Lösung/ Unsymmetrically Substituted Phosphino Sulfur Diimides – NMR Studies on the Configuration in Solution

Abstract

Komplexe mit aromatischen Carbonsäuren, IV. Ca2[C6H2(COO)4]·6H2O - Eine neue Schichtstruktur/ Complexes with Aromatic Carboxylic Acids, IV. Ca2[C6H2(COO)4]·6H2O - A Novel Layer Structure

Abstract

Darstellung von Dichalkogenostibanen des Typs RSb(ER′)2 (R = CH3, C2H5; E = S, Se; R = CH3, C6H5)/ Preparation of Dichalcogenostibanes of the Type RSb(ER′)2 (R = CH3, C2H5; E = S, Se; R′ = CH3, C6H5 )

Abstract

Zur Stereochemie des freien Elektronenpaares in AX6E-Systemen, VIII. Statisch verzerrte Anionen in [H3N(CH2)3NH3]3(BiX6)2(H2O)2 mit X = Cl, Br/ On the Stereochemistry of the Lone-Pair Electrons in AX6E-Systems, VIII Statically Distorted Anion in [H3N(CH2)3NH3]3(BiX6)2(H2O)2 with X = Cl, Br

Abstract

Triazaphosphinine – Reaktionen, Zwitterionen, P–B-Austausch/ Triazaphosphinines – Reactions, Zwitter Ions, P – B-Exchange

Abstract

NaGaSn5, eine neue Zintl-Phase mit Ga–Sn-Schrauben/ NaGaSn5, a New Zintl Phase Containing Ga–Sn Helices

Abstract

Synthese und Eigenschaften von tert-Butyltriiodsilan/ Synthesis and Properties of tert-Butyltriiodosilane

Abstract

Zur Polymorphie von TbCI3/ Polymorphism of TbCl3

Abstract

Synthese und Kristallstruktur von (Cyclopentadienyl)(dicarbonyl)(1,5-di-/Molyl-pentaazadienido)molybdän, (Cp)Mo(CO)2(tolN5tol)/ Synthesis and Crystal Structure of (Cyclopentadienyl)(dicarbonyl)(1,5-di-p-tolyl-pentaazadienido)molybdenum, (Cp)Mo(CO)2(tolN5tol)

Abstract

[Fe(phen)3]2Sb6l22·2CH3CN: Ein Iodoantimonat mit zentralem [Sb6I6]-Doppelwürfel (phen = 1,10-Phenanthrolin)/ [Fe(phen)3]2Sb6I22 · 2 CH3CN: An Iodoantimonate with Central [Sb6I6]-Double Cube (phen = 1,10-Phenanthrolin)

Abstract

Synthesis and Activity of Juvenile Hormone Analogues (JHA)

Abstract

meso-Substituierte Porphyrine, 5. Korbporphyrine meso-Substituted Porphyrins, 5. Basket Porphyrins

Abstract

The Crystal Structure of Potassium Nickel Arsenate; KNiAsO4

Abstract

Nicotinamide Nucleotides in Different Types of Human Cataractous Lenses

Abstract

The Structure and Absolute Configuration of Cyclotirucanenol, a New Triterpene from Euphorbia tirucalli Linn

Abstract

Ceramid-1-phosphoethanolamine aus Myxococcus stipitatus/ Ceramide-1-phosphoethanolamines from Myxococcus stipitatus

Abstract

Notizen: Synthese und Kristallstruktur von PPh3Me[HSO4]/ Synthesis and Crystal Structure of PPh3Me[HSO4]

Abstract

Notizen: High-field (500 MHz) 1H NMR Spectra of Retinoic Acids and Arotinoids by Two-dimensional Chemical Shift Correlation (2D) Spectroscopy

Abstract

[Fe(CO)₄C(O)NMe₂][C(NMe₂)₃]; die erste Strukturbestimmung einer Organometallverbindung mit dem Carbeniumion [C(NMe₂)₃]⁺/ [Fe(CO)₄C(O)NMe₂][C(NMe₂)₃]; the First Structure Determination on an Organometallic Compound with the Carbenium Ion [C(NMe₂)₃]⁺

Über die Reaktion von Dicyan mit Cd(II)-Ionen Röntgenstrukturanalyse von [Cd{(CN)₂}₂SO₂ ][AsF₆]₂/ The Reaction of Cyanogen with Cd(II) Ions X-Ray Structure Analysis of [Cd{(CN)₂}₂SO₂][AsF₆]₂

Synthese, Eigenschaften und Kristallstruktur von (NH₄)NbOBr₄/ Synthesis, Properties and Crystal Structure of (NH₄)NbOBr₄

Komplexe mit aromatischen Carbonsäuren, IV. Ca₂[C₆H₂(COO)₄]·6H₂O - Eine neue Schichtstruktur/ Complexes with Aromatic Carboxylic Acids, IV. Ca₂[C₆H₂(COO)₄]·6H₂O - A Novel Layer Structure

Darstellung von Dichalkogenostibanen des Typs RSb(ER′)₂ (R = CH₃, C₂H₅; E = S, Se; R = CH₃, C₆H₅)/ Preparation of Dichalcogenostibanes of the Type RSb(ER′)₂ (R = CH₃, C₂H₅; E = S, Se; R′ = CH₃, C₆H₅ )

NaGaSn₅, eine neue Zintl-Phase mit Ga–Sn-Schrauben/ NaGaSn5, a New Zintl Phase Containing Ga–Sn Helices

Zur Polymorphie von TbCI₃/ Polymorphism of TbCl₃

Synthese und Kristallstruktur von (Cyclopentadienyl)(dicarbonyl)(1,5-di-/Molyl-pentaazadienido)molybdän, (Cp)Mo(CO)₂(tolN₅tol)/ Synthesis and Crystal Structure of (Cyclopentadienyl)(dicarbonyl)(1,5-di-p-tolyl-pentaazadienido)molybdenum, (Cp)Mo(CO)₂(tolN₅tol)

[Fe(phen)₃]₂Sb₆l₂₂·2CH₃CN: Ein Iodoantimonat mit zentralem [Sb₆I₆]-Doppelwürfel (phen = 1,10-Phenanthrolin)/ [Fe(phen)₃]₂Sb₆I₂₂ · 2 CH₃CN: An Iodoantimonate with Central [Sb₆I₆]-Double Cube (phen = 1,10-Phenanthrolin)

The Crystal Structure of Potassium Nickel Arsenate; KNiAsO₄

Notizen: Synthese und Kristallstruktur von PPh₃Me[HSO₄]/ Synthesis and Crystal Structure of PPh₃Me[HSO₄]

Notizen: High-field (500 MHz) ¹H NMR Spectra of Retinoic Acids and Arotinoids by Two-dimensional Chemical Shift Correlation (2D) Spectroscopy