Published by De Gruyter

Volume 41 Issue 7

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Synthese, Molekül-und Kristallstruktur von 3,5-Dimethyl-2,6-bistrimethylsilyl- 1-thia-2,4,6-triaza-3,5-diborinan-wolframpentacarbonyl/ Synthesis, Molecular and Crystal Structure of 3,5-Dimethyl-2,6-bistrimethylsilyl- 1-thia-2,4,6-triaza-3,5-diborinane-tungstenpentacarbonyl

Carl Habben, Anton Meller, Matthias Noltemeyer, George M. Sheldrick

Page range: 799-802

More Download PDF

Abstract

The am monolysis of 3,5-dim ethyl-2,6-bistrimethylsilyl-1,4-dithia-2,6-diaza-3,5-diborinane leads to 3,5-dim ethyl-2,6-bistrim ethylsilyl-1-thia-2,4,6-triaza-3,5-diborinane, which reacts with tungstenpentacarbonyl · TH F to give the title-com pound. 1 H , 11 B , 13 C, 14 N , 29 Si NMR spectra, IR and MS data, and the results of an X-ray analysis are reported.

Open Access June 2, 2014

Darstellung und Kristallstrukturen von [Ph₄As⁺][PS₂(N₃)₂] und [(n-C₃H₇)₄N⁺]₂[(NCPS₂)₂S^2-]/ Preparation and Crystal Structures of [Ph₄As⁺][PS₂(N₃)₂^–] and [(n-C₃H₇)₄N⁺]₂ [(NCPS₂)₂S₂^–]

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

Page range: 803-807

More Download PDF

Abstract

The diazidodithiophosphate anion [PS 2 (N 3 ) 2 - ] can be isolated with a large cation as (Ph 4 As + ][PS 2 (N 3 ) 2 - ] (1). [PS 2 (N 3 ) 2 - ] is formed by the reaction of P 4 S 10 with NaN 3 in acetonitrile as a solvent. [(NCPS 2 ) 2 S 2 - ] results from the reaction of P 4 S 10 with NaCN in acetonitrile and is isolated as [(n-C 3 H 7 ) 4 N + H(NCPS 2 ) 2 S 2- ] (2). 1 crystallizes in the triclinic space group P1̄ with a - 1329.3(3), b = 1419.1(3),c = 2182.3(5) pm, α = 71.71(2), β = 87.21(2), γ = 84.97(2)° and Z = 6. Crystals of 2 are monoclinic, space group P2 1 /n, a - 1899.0(3), b - 949.0(2), c = 2128.4(5) pm, β = 112.90(2)°, Z = 4.

Open Access June 2, 2014

Kurze inter-und intramolekulare W asserstoffbrückenbindungen in sauren Salzen halogensubstituierter Orthophthalsäuren/ Short Inter-and Intramolecular Hydrogen Bonds in Acid Salts of Halogen-Substituted o-Phthalic Acids

Rainer Mattes, Angela Dorau

Page range: 808-814

More Download PDF

Abstract

The hydrogen bonding in several acid salts of 4,5-dichlorophthalic, 3,6-dichlorophthalic and 3-fluorophthalic acid have been studied by IR spectroscopy and X-ray structure analysis. NH 4 H [3,6-Cl 2 C 8 H 2 O 4 ] and KH[3-FC 8 H 3 O 4 ], with O···O distances of 247 and 254.1(4) pm, respectively, belong to Speakman’s type B 2 of acid salts of dicarboxylic acids. In NH 4 H[4,5-Cl 2 C 8 H 2 O 4 ] · H 2 O a short hydrogen bond of 253(1) pm is formed to the H 2 O molecule. A very short intramolecular hydrogen bond of only 234.0(10) pm length was found in N(C 4 H 9 ) 4 H[4,5-Cl 2 C 8 H 2 O 4 ], In the [3,6-Cl 2 C 8 H 2 O 4 ] 2- dianion both carboxylate groups are nearly orthogonal to the phenyl ring.

Open Access June 2, 2014

Zur Frage der nicht-enzymatischen Bildung von kondensierten Phosphaten unter präbiotischen Bedingungen/ Non-Enzymatic Formation of Condensed Phosphates under Prebiotic Conditions

F. Seel, K.-P. Klos, D. Recktenwald, J. Schuh

Page range: 815-824

More Download PDF

Abstract

One of the problems of chemical evolution on the primitive Earth is the question of the possibility of a non-enzymatic spontaneous condensation o f phosphoric acid and hydrogen phosphates to yield polyphosphoric acids and polyphosphates in aqueous system s, by means of which phosphorus might have entered into early metabolisms. The extra- or intra-cellular formation of magnesium diphosphate under geologically plausible hydrothermal conditions from either magnesium hydrogen phosphates or calcium phosphates in media has been demonstrated.

Open Access June 2, 2014

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh₄)₂ [ReBr₄(NS)(NSBr)]·CH₂Br₂ Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh₄)₂[ReBr₄(NS)(NSBr)]·CH₂Br₂

Hans-Günter Hauck, Wolfgang Willing, Ulrich Müller, Kurt Dehnicke

Page range: 825-830

More Download PDF

Abstract

The thionitrosyl-halothionitrene com pounds (PPh 4 ) 2 [ReX 4 (NS)(NSX)]·2 CH 2 X 2 , X = Cl or Br, are obtained by nucleophilic ring cleavage of the Re(N 2 S 2 ) rings of complexes [ReX 4 (N 2 S 2 )] ⊖ with PPh 4 X in CH 2 X 2 . (AsPh 4 ) 2 [ReCl 4 (NS)(NSCl)] · CH 2 Cl 2 can also be obtained by the reaction of [ReCl 4 (NSCl)(POCl 3 )] with S(NSiMe 3 ) 2 and subsequent addition of AsPh 4 Cl. The pyridine complex [ReBr 2 (NS)(NSBr)(NC 5 H 5 ) 2 ] · CH 2 Br 2 forms by bromination of the corresponding chloro compound with Me 3 SiBr. The IR spectra are reported. The crystal structure of (PPh 4 ) 2 [ReBr 4 (NS)(NSBr)] · CH 2 Br 2 was determ ined by X-ray diffraction (4158 independent observed reflexions, R = 0.059). Crystal data: a = 1039.7, b - 1232.5, c - 2158.4 pm, α = 81.59, β = 87.05, γ = 77.06°, Z = 2, space group P1̄. The compound consists of PPh 4 ⊕ ions, CH 2 Br 2 molecules, and anions [ReBr 4 (NS)(NSBr)] 2⊖ in which the rhenium atoms are coordinated by four bromine atoms, one thionitrosyl and one brom othionitrene group. The latter have cis arrangement and ReN bond lengths of 186 pm. W hereas the thionitrosyl group is nearly linear, the R = N = SBr group has an ReNS angle of 165°.

Open Access June 2, 2014

Synthese und Kristallstruktur von VBr₂(N₃S₂)(Pyridin)₂/ Synthesis and Crystal Structure of VBr₂(N₃S₂)(pyridine)₂

Wolfgang Willing, Ruth Christophersen, Ulrich Müller, Kurt Dehnicke

Page range: 831-833

More Download PDF

Abstract

VBr 2 (N 3 S 2 )(pyridine) 2 is obtained in form of brown-black, moisture sensitive crystals by the reaction of the corresponding chloro complex with trim ethylbrom osilane. The com pound is characterized by its IR spectrum and an X-ray crystal structure determination (1322 observed reflexions, R = 0.077). Crystal data: monoclinic, space group Aba2, Z = 4, a = 1100.3, b = 1480.0, c = 983.3 pm. A molecular structure with a distorted octahedral coordination for the vanadium atoms was found: there are two short VN bonds o f 178 pm with two N atoms o f the planar N 3 S 2 chelate, two long (228 pm) VN(pyridine) bonds trans to the former VN bonds and two bromo ligands.

Open Access June 2, 2014

Bis[tetraethylammonium]-meso-bis[dichloro-μ-chloro-oxo-aquavanadat(IV)], [(C₂H₅)₄N]₂[{VOCl₂(OH₂)}₂(μ-Cl)₂]: Molekülstruktur und spektroskopische Charakteristika/ Tetraethylammonium raeso-Bis[dichloro-μ-chloro-oxo-aquavanadate(IV)], [(C₂H₅)₄N]₂[{VOCl₂(OH₂)}₂(μ-Cl)₂]: Molecular Structure and Spectroscopic Characteristics

Wolfgang Priebsch, Carola Weidemann, Dieter Rehder, Jürgen Kopf

Page range: 834-838

More Download PDF

Abstract

The title compound crystallizes in the monoclinic space group P2 1 /c with a = 822.0(1), b = 1126.4(2), c = 1629.0(2) pm and β = 103.54(1)°. The two vanadium centers of the anion, which is an edge-bridged bioctahedron, are asymmetrically connected by bridging chloroligands; V -(μ -Cl) bond lengths are 238.4 und 278.3 pm , respectively. ESR and IR characteristics are discussed.

Open Access June 2, 2014

1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl₂PN₂CCl]₃, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl₂PN₂CCl]₃, Preparation, Spectra and Crystal Structure

H .-D. Hausen, G. Rajca, J. Weidlein

Page range: 839-844

More Download PDF

Abstract

The title compound, Cl 2 PN 2 CCl, has been synthesized by the reaction of PCl 5 with Me 3 Si -N = C = N - SiMe 3 (Me - CH 3 ) in a 1:1 molar ratio. The colourless com pound is trimericin benzene solution and in the solid state and has a structure with a highly puckered 12-membered P 3 N 6 C 3 -ring skeleton of low symmetry. The X-ray structure determination shows a monoclinic space group P 2 1 /a with 4 trimeric units per cell.

Open Access June 2, 2014

Beiträge zur Chemie der Carbonylkomplexe mit Germanium-bzw. Zinn-Übergangsmetall-Bindungen/ Contributions to the Chemistry of Carbonyl Complexes with Germanium or Tin Transition Metal Bonds

Helmut Behrens, Matthias Moll, Peter Merbach, Karl-Heinz Trümmer

Page range: 845-851

More Download PDF

Abstract

Dihalogeno bis(carbonylm etalato) germanium (IV) and tin(IV ) com pounds listed in Table I are obtained in high yields by the reaction o f TlCo(CO) 4 or TlFe(CO) 3 NO with trihalogeno carbonylmetalato germanium(IV) and tin(IV) complexes. The new com pounds are characterized by their analyses, mass and vibrational spectra.

Open Access June 2, 2014

Kristallstrukturen von NaMg₂OH(SO₃)₂ · H₂O, NaMn₂OH(SO₃)₂ · H₂O , NaFe₂OH(SO₃)₂ · H₂O, NaCo₂OH (SO₃)₂ H₂O und NaZn₂OH(SO₃)₂H₂O/ Crystal Structures of NaMg₂OH(SO₃)2-H₂O, NaMn₂OH(SO₃)₂ · H₂O,NaFe₂OH(SO₃)₂H₂O, NaCo₂OH(SO₃)₂ · H₂O, and NaZn₂OH(SO₃)₂ · H₂O

Willi Buchmeier, Bernward Engelen, Heinz Dieter Lutz

Page range: 852-858

More Download PDF

Abstract

The crystal structures of the isotypic hydroxosulfitometalates NaM 2 OH(SO 3 ) 2 ·1H 2 O with M = Mg, Mn, Fe, Co, and Zn were determined by means of X-ray single crystal data (triclinic space group P1̄ - Q i 1 , Z = 2). The final R for the 2223, 2496, 2440, 1461, and 3433 observed reflections are 0.043, 0.068, 0.025, 0.055, and 0.028, respectively. The bivalent metal ions (three types) are octahedrally coordinated by the oxygen atoms of adjacent SO 3 2- ions (two types, both monodentate), OH - groups, and water molecules. The arrangement of the two OH - groups is trans, and of OH - and H 2 O cis with respect to the octahedral coordination. The mean metal oxygen distances are in the order M - OH 2 > M -OSO 2 2- > M - OH . The MO 6 -octahedra are both vertex and edge sharing, forming two-dimensional networks parallel to (010), which are connected via hydrogen bonds. The water molecules form strong, linear, nearly symmetric (mm 2) hydrogen bonds to SO 3 2- ions, the hydroxide ions weak bonds to water molecules.

Open Access June 2, 2014

Diphenyl[mono(per)fluoracyI- und aroyl(oxy)]phosphan(oxid)e – neue Synthesen, neue Verbindungen/ Diphenyl[mono(per)fluoroacyl- and aroyl(oxy)]phosphan(oxid)es – New Synthetic Methods, New Compounds

Heinz-Werner Hennig, Peter Neu, Peter Sartori

Page range: 859-862

More Download PDF

Abstract

Diphenylpentafluorobenzoyloxyphosphane 2 a was prepared by reacting diphenylchlorophosphane with sodium pentafluorobenzoate. Reaction of diphenylchlorophosphane with sodium salts of trifluoroacetic acid and of 4-ethoxy-2,3,5,6-tetrafluorobenzoic acid leads to diphenyl trifluoroacetyl phosphane oxide 3b and to diphenyl 4-ethoxy-2,3,5,6-tetrafluoro benzoyl phosphane oxide 3 e. IR data, 19 F and 31 P { 1 H } NMR data are given.

Open Access June 2, 2014

Chemie polyfunktioneller Moleküle, 98. Oxidative Ringerweiterung des P₃-Nortricyclans, 4-Methyl-1,2,6-triphosphatricycIo[2.2.1.0^2,6]heptan, mit Schwefel und Selen zu Hetero-Noradamantanen und -Adamantanen/ Chemistry of Polyfunctional Molecules, 98. Oxidative Ring Enlargement of the P₃-Nortricyclane, 4-Methyl-1,2,6-triphosphatricyclo- [2.2.1.0^2,6]heptane, by Sulfur and Selenium to Hetero Noradamantanes and Adamantanes

Jochen Ellermann, Alfons A. M. Demuth, Walter Bauer

Page range: 863-869

More Download PDF

Abstract

4-Methyl-1,2,6-triphosphatricyclo[2.2.1.0 2.6 ]heptane, CH 3 C(CH 2 P) 3 (1) reacts with sulfur or selenium in the molar ratios of 1:3, 1:5 and 1:6 to yield the chalcogeno-dichalcogenatriphosphanoradamantanes CH 3 C (CH 2 P) 3 E 2 (E ) (E = S, Se; 2a, b), the dichalcogeno-trichalcogenatriphospha- adamantanes CH 3 C(CH 2 PE) 3 (E) 2 (E = S, Se; 3a, b) and the trichalcogeno-trichalcogenatriphospha- adam antanes CH 3 C(CH 2 PE) 3 (E ) 3 (E = S, Se; 4a, b). The selenium derivative 4b could be detected only by 31 P{ 1 H} NM R spectroscopy. Main product in the 1:6 reaction of 1 with selenium is 3b.

Open Access June 2, 2014

Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LII. Bindungs- und Strukturverhältnisse von Phosphidocobaltaten in Lösung und im festen Zustand/ Preparation and Properties of, and Reactions with, Metal-Containing Heterocycles, LII. Bonding and Structural Conditions of Phosphidocobaltates in Solution and in Solid State

Ekkehard Lindner, Petra Neese

Page range: 870-876

More Download PDF

Abstract

Reduction of [(OC) 3 CoPPh 2 ] n (1a ) with excess sodium granules affords [(OC) 3 CoPPh 2 ]Na 2 (3a) in solution as well as in solid state. However, in analogous reactions of [(OC) 3 CoPR 2 H] 2 (1b : R = C 6 H 11 ; 1c : R = t-Bu) with excess sodium granules the monovalent anionic complexes [(OC) 3 CoPR 2 H]Na (2b, c) are obtained in THF solution. 2b, c cannot be isolated in solid state. After removal of THF from their solutions the purified residues were identified by elemental analyses as [(OC) 3 CoPR 2 ]Na 2 (3b, c). Addition of buthyllithium to THF solutions of 3a, 2b, c gives rise to differently solvated complexes 3a*-c* which are transformed to [(OC) 3 CoPR 2 ]M 2 (M = N a, Li; 3 a′-c′). The course of the reactions and the products are controlled IR and 31 PNMR spectroscopically. 2b, c and 3a, b′, c′ were trapped with (H 3 CO) 2 SO 2 and CH 2 X 2 (X = Cl, I) yielding H 3 CCo(CO) 3 PR 2 H(6b, c), H 3 CCo(CO) 3 PR 2 CH 3 (4a - c ) and [xxx] (5a, b), respectively.

Open Access June 2, 2014

Übergangsmetallkomplexe mit Schwefelliganden, XVIII. Synthese und Reaktionen von [Ru(L)(PPh₃)dttd]-Komplexen mit kleinen Stickstoffverbindungen L = NH₃, N₂H₄, N₂H₃CH₃, N₂H₃C₆H₅ sowie NO⁺ (dttd^2- = 2,3;8,9-Dibenzo-1,4,7,10-tetrathiadecan (–2))/ Transition Metal Complexes with Sulfur Ligands, XVIII. Synthesis and Reactions of [Ru(L)(PPh₃)dttd] Complexes with Small Nitrogen Compounds L = NH₃, N₂H₄, N₂H₃CH₃, N₂H₃C₆H₅ and NO⁺ (dttd^2- = 2,3;8,9-Dibenzo-1,4,7,10-tetrathiadecane (–2))

Dieter Sellmann, Michael Waeber

Page range: 877-884

More Download PDF

Abstract

Reaktionen von [Ru(L)(PPh3)dttd]-Komplexen mit kleinen Stickstoffverbindungen L = NH3, N2H4, N2H3CH3, N2H3C6H5 sowie NO+ (dttd2-= 2,3;8,9-Dibenzo-l,4,7,10-tetrathiadecan (—2)) Transition Metal Complexes with Sulfur Ligands, XVIII* Synthesis and Reactions of [R u(L)(PPh3)dttd] Complexes with Small Nitrogen Com pounds L = N H 3, N2H 4, N2H 3C H 3, N2H 3C6H 5 and N O + (dttd2-= 2,3;8,9-D ibenzo-l,4,7,10-tetrathiadecane (—2)) D ieter Sellmann+ Ruthenium Sulfur C om plexes, N itrogen Ligands The com plex fragment [Ru(PPh3)dttd], (dttd2-= 2,3;8,9-dibenzo-l,4,7,10-tetrath iad ecane (— 2)), coordinates small nitrogen com pounds, which have only o-as well as a-jr-donor proper ties. The reactions o f [Ru(PPh3)2dttd] with L — N H 3, N 2H 4, N 2H 3C H 3 and N 2H 3C6H 5, respec tively, give the corresponding [R u(L)(PP h3)dttd] com plexes. O xidation o f the hydrazine com plex [R u(N 2H 4)(PPh3)dttd] yields [a-N 2H 2{R u(PP h3)dttd }2], the first diazene com plex in which the unstable N 2H 2 is bound to a sulfur coordinated m etal center and stabilized by a 4 c —6 e Ru— N — N — Ru system , steric shielding as well as thiolate — S---H (n,h2)---N hydrogen bridges. The reactions of the ammonia and the hydrazine com plexes, respectively, with N O PF6 yield the nitrosyl com plex [R u (N O)(PP h3)dttd]PF6 as final product; in the case o f [R u(N 2H 4)(P P h3)dttd] the intermediate formation of an azido com plex is observed IR -spectroscopically.

Open Access June 2, 2014

Darstellung und Schwingungsspektren von Fluoro-Chloro-Osmaten(V)/ Preparation and Vibrational Spectra of Fluoro-Chloro-Osm ates(V)

W. Preetz, Th. Groth

Page range: 885-889

More Download PDF

Abstract

By oxidation of the pure fluoro-chloro-osmates(IV ) with BrF 3 in dichlorom ethane the mixed pentavalent complexes [OsF 5 Cl] - , cis-[OsF 4 Cl 2 ] - , fac-[OsF 3 Cl 3 ] - and cis-[OsF 2 Cl4] - are formed without replacement of ligands. Trans-[OsF 4 Cl 2 ] - and trans-[OsF 2 Cl 4 ] - are generated from the corresponding osmates(IV) by oxidation with PbO 2 in dichloromethane under addition of trifluoroacetic acid. The vibrational spectra o f the mixed ligand complexes are assigned according to point groups D 4h , C 4v , C 3v and C 2v . The increased bond strength com pared with the corresponding Os(IV ) complexes is indicated by a significant shift to higher energy by about 5 -15% . The Os -Cl stretching vibration of [OsF 5 Cl] - and also the symmetric ClOsCl of trans-[OsF 4 Cl 2 ] - is split by the isotopes 35 Cl and 37 Cl, showing two and three well resolved sharp Raman lines in the expected ratio of intensities, respectively.

Open Access June 2, 2014

Organoborierung von Alkinylstannanen, XVIII. Neue kondensierte heterocyclische Systeme aus N- und C-lithiierten Azolen und cis- 1,2-organometallisch substituierten Alkenen/ Organoboration of Alkynylstannanes, XVIII. Novel Fused Heterocyclic Systems from N- and C-Lithiated Azoles and cis-1,2-Organometallic Substituted Alkenes

Susanna Kerschl, Bernd Wrackmeyer

Page range: 890-894

More Download PDF

Abstract

Organoboration of dimethyl(chloro)-1-propynylstannane with triethylborane gives (E̲)-2-dimethyl(chloro)stannyl-3-diethylboryl-pent-2-ene (2a) in high yield. Reactions of 2a with N- and C-lithiated azoles (pyrazole, 1-m ethylimidazole, 1-methyl-1,2,4-triazole) lead to the new fused heterocyclic systems 8, 10, 12. In the case of 10 and 12 it was possible to detect (by 11 B, 119 Sn NM R ) the isomers 9 and 11 which have a zwitterionic structure with an Sn-N linkage. After heating, the compounds 9 and 11 rearrange quantitatively into 10 and 12, respectively. These results show the com petition between boron and tin in 2a as electrophilic centres.

Open Access June 2, 2014

Interpretation of Substituent Angular Parameters of Monosubstituted Benzenes by Means of ab initio STO-3G Fully Optimized Molecular Structures and Charges Densities. Part VI of the Series: “Crystallographic Studies and Physicochemical Properties of π-Electron Systems”

Tadeusz Marek Krygowski, Günter Häfelinger, Josef Schüle

Page range: 895-903

More Download PDF

Abstract

The angular variations of molecular structures calculated for 17 monosubstituted derivatives of benzene by use of ab initio analytical gradient optimization at the STO -3G level have been correlated by multiple linear regression analysis with Mulliken σ- and π-electron charge densities at corresponding ring carbon atoms. Variations of angles γ at meta positions are solely due to π-electron effects (R = 0.961). Changes in angles β at ortho positions are independent of σ- or π-electron effects but may be related to steric effects (R = 0.719) alone or additionally to charge densities on ortho protons (for dual regression R = 0.846). Angles a at ipso atom s depend significantly on both, σ- and π-electron charge densities in the ratio of 70% to 21% with R = 0.974 for dual regression. Variations of angles δ para-positions depend on all three effects considered (with correlation coefficient for a triple regression R = 0.951) in the ratio 37.6% :2 8 .3% : 34.1% for steric effects, σ- and π-electron charge densities, respectively.

Open Access June 2, 2014

Die Photoreaktion von Re₂(CO)₁₀ mit Ethylen und Ethylenderivaten/ The Photoreaction of Re₂(CO)₁₀ with Ethylene and Ethylene Derivatives

Cornelius G. Kreiter, Karl Heinz Franzreb, William S. Sheldrick

Page range: 904-914

More Download PDF

Abstract

Re 2 (CO) 10 (1) has been photolyzed at reduced temperature in the presence of ethylene (2), styrene (3) or 2-methyl-1,3-butadiene (4), respectively. Main products of these reactions are the octacarbonyl-μ-hydrido-μ-η 2:1 -olefinyl-dirhenium (6, 9, 12, 13, 15) and tridecacarbonyl-μ-η 2:1 - olefinyl-trirhenium complexes (7, 14, 16). In lesser amounts, three isomeric undecacarbonyl-μ- hydrido-bis(μ-η 2:1 -vinyl)trirhenium com pounds (8 a, 8 b, 8 c), enneacarbonyl-η 2 -ethylenedirhenium (5) and three octacarbonyl-η 4 -diene-dirhenium complexes (10,17,18) are formed. The reaction products were separated by HPL chromatography. They were characterized by IR and NM R spectroscopy ( 1 H , 13 C) and by C, H elemental analyses. The molecular and crystal structure of tridecacarbonyl-η 2:1 -E-3-methyl-1,3-butadien-1-yl-trirhenium was determined by X-ray structure analysis.

Open Access June 2, 2014

Phosphorverbindungen ungewöhnlicher Koordination, 13. Abfangreaktionen von Phenyl-thioxophosphan durch [4+1]-CycIoaddition mit o-Chinonen/ Phosphorus Compounds with Unusual Coordination, 13 [1] Trapping Reactions of Phenyl Thioxophosphane by [4+1] Cycloaddition with o-Quinones

Rita Hussong, Heinrich Heydt, Manfred Regitz

Page range: 915-921

More Download PDF

Abstract

Phenyl thioxophosphane (1) - generated by thermal cycloreversion from 7 along with the dihydropyridazine 8 - is trapped by [4+1] cycloaddition with the o-quinones 9a-f by formation of the dioxaphospholsulfides 10a-f. Solvolysis of 10a-c, e and f with m ethanol yields the phenol derivatives 12a-e (in the case of 10b the isomer 12b′ is formed, too). This reaction is reversible (12a-c→10a-c) and accompanied by formation of the isomers 13a-c. The phenanthrene quinone methanide 14 is also suitable for the trapping reaction of 1 (→15→17).

Open Access June 2, 2014

Studies on the Chemical Constituents of Azadirachta indica A. Juss (Meliaceae), Part VII

Salimuzzaman Siddiqui, Shaheen Faizi, Bina Shaheen Siddiqui

Page range: 922-924

More Download PDF

Abstract

A new limonoid, nim bocinol, has been isolated from the fresh, undried, ripe fruits of Azadirachta indica (neem ) along with known com ponents, azadirone, epoxyazadiradione, azadiradione, gedunin, 17-hydroxyazadiradione and cholesterol. It is the first report of the isolation of cholesterol from any part of the neem tree.

Open Access June 2, 2014

Studies on Heterocyclic Enamines: New Synthesis of Pyrano[2,3-b]pyndine, Pyrano[2,3-d]pyrimidine and Pyrano[2,3-c]pyrazole Derivatives

Nosrat Mustafa Abed, Nadia Sobhy Ibrahim, Mohamed Helmy Elnagdi

Page range: 925-928

More Download PDF

Abstract

A variety of novel pyrano[2,3-d]pyrimidines could be obtained via reaction of ethyl 2-amino- 3-cyano-6-methylpyran-4-carboxylate with a variety of reagents. Evidence for the existance of this pyran derivative as a ring chain tautom er is presented.

Open Access June 2, 2014

Notizen: Eine neue Synthese und das IR-Spektrum von [SNBr_0,4]_x/ A New Synthesis and the IR Spectrum of [SNBr_0,4]_x

Udo Demant, Kurt Dehnicke

Page range: 929-930

More Download PDF

Abstract

[SNBr 0,4 ] x was prepared by the reaction of trithiazyl chloride with BrSiMe 3 in CH 2 Cl 2 solution at -60 °C. The IR spectrum is recorded and discussed. The mass spectrum is in agreement with samples prepared by other pathways.

Open Access June 2, 2014

Notizen: Phosphorverbindungen ungewöhnlicher Koordination, 12. Diels-Alder-Reaktionen mit ^tBu–C ≡ P – ein ergiebiger Weg zu λ₃-Phosphininen/ Phosphorus Compounds with Unusual Coordination, 12. Diels-Alder Reactions with ^tB u–C≡ P–a Lucrative Access to λ³-Phosphinines

Wolfgang Rösch, Manfred Regitz

Page range: 931-934

More Download PDF

Abstract

Diels-Alder reactions of the phosphaalkyne 4 with the cyclic 1,3-dienes 5 generate the adducts 6 which decompose spontaneously under elimination of “X ” to yield the λ 3 -phosphinines 7. The bicyclic 9 decomposes into 7b on flash pyrolysis

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)

> Information on submission process

Volume 41 Issue 7

Issue of Zeitschrift für Naturforschung B

Synthese, Molekül-und Kristallstruktur von 3,5-Dimethyl-2,6-bistrimethylsilyl- 1-thia-2,4,6-triaza-3,5-diborinan-wolframpentacarbonyl/ Synthesis, Molecular and Crystal Structure of 3,5-Dimethyl-2,6-bistrimethylsilyl- 1-thia-2,4,6-triaza-3,5-diborinane-tungstenpentacarbonyl

Abstract

Darstellung und Kristallstrukturen von [Ph4As+][PS2(N3)2] und [(n-C3H7)4N+]2[(NCPS2)2S2-]/ Preparation and Crystal Structures of [Ph4As+][PS2(N3)2–] and [(n-C3H7)4N+]2 [(NCPS2)2S2–]

Abstract

Kurze inter-und intramolekulare W asserstoffbrückenbindungen in sauren Salzen halogensubstituierter Orthophthalsäuren/ Short Inter-and Intramolecular Hydrogen Bonds in Acid Salts of Halogen-Substituted o-Phthalic Acids

Abstract

Zur Frage der nicht-enzymatischen Bildung von kondensierten Phosphaten unter präbiotischen Bedingungen/ Non-Enzymatic Formation of Condensed Phosphates under Prebiotic Conditions

Abstract

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh4)2 [ReBr4(NS)(NSBr)]·CH2Br2 Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)]·CH2Br2

Abstract

Synthese und Kristallstruktur von VBr2(N3S2)(Pyridin)2/ Synthesis and Crystal Structure of VBr2(N3S2)(pyridine)2

Abstract

Abstract

1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl2PN2CCl]3, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl2PN2CCl]3, Preparation, Spectra and Crystal Structure

Abstract

Beiträge zur Chemie der Carbonylkomplexe mit Germanium-bzw. Zinn-Übergangsmetall-Bindungen/ Contributions to the Chemistry of Carbonyl Complexes with Germanium or Tin Transition Metal Bonds

Abstract

Kristallstrukturen von NaMg2OH(SO3)2 · H2O, NaMn2OH(SO3)2 · H2O , NaFe2OH(SO3)2 · H2O, NaCo2OH (SO3)2 H2O und NaZn2OH(SO3)2H2O/ Crystal Structures of NaMg2OH(SO3)2-H2O, NaMn2OH(SO3)2 · H2O,NaFe2OH(SO3)2H2O, NaCo2OH(SO3)2 · H2O, and NaZn2OH(SO3)2 · H2O

Abstract

Diphenyl[mono(per)fluoracyI- und aroyl(oxy)]phosphan(oxid)e – neue Synthesen, neue Verbindungen/ Diphenyl[mono(per)fluoroacyl- and aroyl(oxy)]phosphan(oxid)es – New Synthetic Methods, New Compounds

Abstract

Abstract

Abstract

Abstract

Darstellung und Schwingungsspektren von Fluoro-Chloro-Osmaten(V)/ Preparation and Vibrational Spectra of Fluoro-Chloro-Osm ates(V)

Abstract

Abstract

Interpretation of Substituent Angular Parameters of Monosubstituted Benzenes by Means of ab initio STO-3G Fully Optimized Molecular Structures and Charges Densities. Part VI of the Series: “Crystallographic Studies and Physicochemical Properties of π-Electron Systems”

Abstract

Die Photoreaktion von Re2(CO)10 mit Ethylen und Ethylenderivaten/ The Photoreaction of Re2(CO)10 with Ethylene and Ethylene Derivatives

Abstract

Phosphorverbindungen ungewöhnlicher Koordination, 13. Abfangreaktionen von Phenyl-thioxophosphan durch [4+1]-CycIoaddition mit o-Chinonen/ Phosphorus Compounds with Unusual Coordination, 13 [1] Trapping Reactions of Phenyl Thioxophosphane by [4+1] Cycloaddition with o-Quinones

Abstract

Studies on the Chemical Constituents of Azadirachta indica A. Juss (Meliaceae), Part VII

Abstract

Studies on Heterocyclic Enamines: New Synthesis of Pyrano[2,3-b]pyndine, Pyrano[2,3-d]pyrimidine and Pyrano[2,3-c]pyrazole Derivatives

Abstract

Notizen: Eine neue Synthese und das IR-Spektrum von [SNBr0,4]x/ A New Synthesis and the IR Spectrum of [SNBr0,4]x

Abstract

Notizen: Phosphorverbindungen ungewöhnlicher Koordination, 12. Diels-Alder-Reaktionen mit tBu–C ≡ P – ein ergiebiger Weg zu λ3-Phosphininen/ Phosphorus Compounds with Unusual Coordination, 12. Diels-Alder Reactions with tB u–C≡ P–a Lucrative Access to λ3-Phosphinines

Abstract

Darstellung und Kristallstrukturen von [Ph₄As⁺][PS₂(N₃)₂] und [(n-C₃H₇)₄N⁺]₂[(NCPS₂)₂S^2-]/ Preparation and Crystal Structures of [Ph₄As⁺][PS₂(N₃)₂^–] and [(n-C₃H₇)₄N⁺]₂ [(NCPS₂)₂S₂^–]

Brom- und Chlorthionitrenkomplexe des Rheniums. Die Kristallstruktur von (PPh₄)₂ [ReBr₄(NS)(NSBr)]·CH₂Br₂ Bromo- and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh₄)₂[ReBr₄(NS)(NSBr)]·CH₂Br₂

Synthese und Kristallstruktur von VBr₂(N₃S₂)(Pyridin)₂/ Synthesis and Crystal Structure of VBr₂(N₃S₂)(pyridine)₂

1,1,3,5,5,7,9,9,11-Nonachlor-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaen: [Cl₂PN₂CCl]₃, Synthese, Spektren und Kristallstruktur/ 1,1,3,5,5,7,9,9,11-Nonachloro-1,5,9-triphospha-2,4,6,8,10,12-hexaazacyclododecahexaene: [Cl₂PN₂CCl]₃, Preparation, Spectra and Crystal Structure

Die Photoreaktion von Re₂(CO)₁₀ mit Ethylen und Ethylenderivaten/ The Photoreaction of Re₂(CO)₁₀ with Ethylene and Ethylene Derivatives

Notizen: Eine neue Synthese und das IR-Spektrum von [SNBr_0,4]_x/ A New Synthesis and the IR Spectrum of [SNBr_0,4]_x

Notizen: Phosphorverbindungen ungewöhnlicher Koordination, 12. Diels-Alder-Reaktionen mit ^tBu–C ≡ P – ein ergiebiger Weg zu λ₃-Phosphininen/ Phosphorus Compounds with Unusual Coordination, 12. Diels-Alder Reactions with ^tB u–C≡ P–a Lucrative Access to λ³-Phosphinines