Published by De Gruyter

Volume 49 Issue 5

Issue of Zeitschrift für Naturforschung B

Contents
Journal Overview

Open Access June 2, 2014

Zur Kristallchemie der Oxoplatinate. Eine neue Phase der Zusammensetzung Sr_4-ϰNa_ϰPtO₆ (ϰ = 0,33) / On the Crystal Chemistry of Oxoplatinates. A New Phase of the Composition Sr_4-ϰNa_ϰPtO₆ (ϰ = 0,33)

G. Tams, Hk. Müller-Buschbaum

Page range: 581-584

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Abstract

Single crystals of Sr 3.67 Na 0 . 33 PtO 6 were prepared by heating oxide mixtures in closed silver tubes and investigated by X-ray single crystal techniques. It crystallizes with trigonal symmetry, space group D 6 3d -R3̅c (Nr. 167) with a = 9.6617, c = 11.6580 Å, Z = 6. Sr 3.67 Na 0 . 33 PtO 6 belongs to the Sr 4 PtO 6 type and is isotypic to K 4 CdCl 6 . One point position characterized by a trigonal prismatic O 2- coordination is occupied by Na + and Sr 2+ statistically. The crystal structure is discussed with respect to the related compounds Sr 3 CuPtO 6 and Ca 3. 5 Cu 0.5 PtO 6 .

Open Access June 2, 2014

Ein Beitrag zur Kristallchemie der oxidischen Alkali-Erdalkali-Edelmetall-Perowskite. Synthese und Kristallstruktur von NaBa₄Cu_0,5Pt_1,5O₈ / A Contribution to the Crystal Chemistry of Alcaline Alealine Earth Precious Metal Perovskites. Synthesis and Crystal Structure of NaBa₄Cu_0,5Pt_1,5O₈

G. Tams, Hk. Müller-Buschbaum

Page range: 585-588

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Abstract

Single crystals of the phase NaBa 4 Cu 0,5 Pt 1,5 O 8 were prepared in closed silver tubes. The black and moisture sensitive crystals were investigated by four-circle diffractometer X-ray techniques. They show trigonal symmetry, space group D 2 3 -P321, a = 10.0644, c = 8.3811 Å, Z = 3 and belong to the perovskites. The typical M 2 C 9 ; double octahedra are occupied by Pt 4+ and Cu 2+ in a different manner. Na + is partly in and out of the centres of trigonal prisms of oxygen. These features will be discussed with respect to the underoccupied point position O(3).

Open Access June 2, 2014

Das erste Oxocuprat/-Arsenat mit Kupfer in gemischter Valenz: Cu(Mg_2,56Cu_0,44)Cu(AsO₄)₃ / The First Oxocuprate/Arsenate Containing Mixed Valent Copper:Cu(Mg_2,56Cu_0,44)Cu(AsO₄)₃

D. Osterloh, Hk. Müller-Buschbaum

Page range: 589-592

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Abstract

Single crystals of Cu(Mg 2 . 56 Cu 0.44 )Cu(AsO 4 ) 3 have been prepared by CO 2 -LASER technique and investigated by X-ray diffraction methods. The light blue crystals show monoclinic symmetry, space group C 6 2h -C2/c, a = 11.897, b = 12.855, c = 6.688 Å, β = 113.06°, Z = 4. The structure type is characterized by AsO 4 tetrahedra, dumb-bell-like coordinated Cu(I), twisted CuO 4 square polygons and octahedra statistically occupied by Mg/Cu 2+ .

Open Access June 2, 2014

μ₂-Halogenokomplexe von N-Bromsuccinimid und N-Bromphthalimid. Die Kristallstrukturen von PPh₄[X(N-Bromsuccinimid)₂] und von PPh₄[X(N-Bromphthalimid)₂] mit X = CI und Br / μ₂-Halogeno Complexes of N-Bromosuccinimide and N-Bromophthalimide. The Crystal Structures of PPh₄ [X(N-Bromosuccinimide)₂] and PPh₄ [X(N-Brom ophthalimide)₂] with X = Cl and Br

Mitra Ghassemzadeh, Klaus Harms, Kurt Dehnicke, Dieter Fenske

Page range: 593-601

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Abstract

The μ2-halogeno complexes PPh 4 [X(N-bromosuccinimide) 2 ] and PPh 4 [X(N-bromophthali- mide) 2 ] with X = Cl and Br have been prepared by reactions of N-bromosuccinimide and N-bromophthalimide, respectively, with the corresponding tetraphenylphosphonium halides PPh 4 X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh 4 [Cl(N-Bromosuccinimide) 2 ] (1): Space group P2 1 /n, Z = 4, structure solution with 2516 observed unique reflections, R = 0.040. Lattice dimensions at -25 °C: a = 1775.9(1), b = 764.3(1), c = 2341.7(2) pm, β = 101.84(1)°. PPh 4 [Br(N-Bromosuccinimide) 2 ] (2): Space group P2 1 /n, Z = 4, structure solution with 5620 observed unique reflections, R = 0.061. Lattice dimensions at 20 °C: a = 1776.9(9), b = 762.2(3), c = 2331(1) pm, β = 103.02(3)°. PPh 4 [Cl(N-Bromophthalimide) 2 ] (3): Space group P1̅, Z = 4, structure solution with 3812 observed unique reflections, R = 0.039. Lattice dimensions at -50 °C: a = 918.5(2), b = 1115.0(3), c = 2584.4(5) pm, α = 88.22(3)°, β = 83.20(3)°, γ = 85.10(3)°. PPh 4 [Br(N-Bromophthalimide) 2 ] (4): Space group P1̅, Z = 2, structure solution with 3413 observed unique reflections, R = 0.044. Lattice dimensions at -50 °C: a = 1120.2(2), b = 1308.6(3), c = 1343.2(3) pm, α = 105.10(3)°, β = 104.16(3)°, γ = 92.99(3)°. The structures of 1-4 consist of PPh 4 + ions, anions [X(N-bromosuccinimide) 2 ] - and [X(N-bromophthalimide) 2 ] - , respectively, in which the halide ions X - are coordinated by the bromine atoms of N-bromosuccinimide and N-bromophthalimide molecules, respectively. The bond angles Br···X···Br are 86.48(5)° for 1, 85.1(1)° for 2, 102.31(6)° and 93.61(6)° for 3, and 91.86(4)° for 4. The bond angles N-Br···X are nearly linear.

Open Access June 2, 2014

μ₂-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh₄[X(N-Iodsuccinimid)₂] · CH₃CN mit X = Cl, Br, / μ₂-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh₄[X(N-Iodosuccinimide)₂] · CH₃CN with X = Cl, Br, I

Mitra Ghassemzadeh, Kurt Dehnicke, Helmut Goesmann, Dieter Fenske

Page range: 602-608

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Abstract

The μ 2 -halogeno complexes PPh 4 [X(N-Iodosuccinimide) 2 ] · CH 3 CN with X = CL Br, I have been prepared by reactions of N-Iodosuccinimide with the corresponding tetraphenylphos- phonium halides PPh 4 X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determinations. PPh 4 [Cl(N-Iodosuccinimide) 2 ] · CH 3 CN (1): Space group Pna2 1 , Z = 4, 4461 observed unique reflections. R = 0.027. Lattice dimensions at -60 °C: a = 1840.5(9), b = 2589(1), c = 728.2(4) pm. PPh 4 [Br(N-Iodosuccinimide) 2 ] · CH 3 CN (2): Space group Pna2 1 Z = 4, 4284 observed unique reflections, R = 0.034. Lattice dimensions at -70 °C: a = 724.8(4), b = 1838.6(9), c = 2601(1) pm. PPh 4 [I(N-Iodosuccinimide) 2 ] · CH 3 CN (3): Space group Pna2 1 , Z = 4, 5775 observed unique reflections. R = 0.031. Lattice dimensions at -60 °C: a = 1849.2(9). b = 2644(1), c = 730.3(4) pm. 1-3 are isotypical. There structures consist of PPh 4 + ions, including acetonitrile molecules without bonding interactions, and anions [X(iodosuccinimide) 2 ] - , in which the halide ions X - are coordinated bv the iodine atoms of the N-iodosuccinimide molecules. The bond angles I··· X···I range from 90.13(4)° (X = Cl) and 88.84(3)° (X = Br) to 87.83(3)° (X = I). The bond angles N- I ··· X are nearly linear.

Open Access June 2, 2014

Benzyliden-und Methylen-bis-silyltriflate als neue Synthesebausteine für Organosiliciumpolymere/ Benzylidene-and Methylene-bis-silyltriflates as New Synthetic Materials for Organosilicon Polymers

W. Uhlig

Page range: 609-614

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Abstract

The title compounds have been prepared by reaction of phenyl-, allyl- or amino-substituted disilylmethanes and disilylphenylmethanes with trifluoromethanesulfonic acid. New organo- silicon oligomers and polymers are obtained in good yields and high purities from these silyltriflates and lithium acetylides, triphenylgermyllithium or diphenylsilanediol/triethylamine. In these compounds the carbosilane units are connected by alkyne or siloxane bridges. The structures have been confirmed by NMR spectroscopy ( 29 Si, 13 C, 1 H) and elemental analysis.

Open Access June 2, 2014

Crystal Structure of Lead(II) Complexes with 2,2'-Iminodiethanol

Alexander V. Sienkiewicz, Vladimir N. Kokozay

Page range: 615-620

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Abstract

The lead(II) complexes of 2,2'-iminodiethanol (H 2 Dea)Pb 2 (Dea)(NO 3 ) 2 (DMF), Pb 2 (HDea) 2 Cl 2 and [Pb 2 Br 6 ](H 3 Dea) 2 (DMF=N,N-dimethylformamide) have been synthesized from the components and characterized by X-ray crystallography. Both mono- (HDea) and doubly (Dea) deprotonated HN(CH 2 CH 2 OH) 2 are coordinated via oxygen and nitrogen atoms in Pb 2 (Dea)(NO 3 ) 2 (DMF) and Pb 2 (TIDea) 2 Cl 2 . The nitrate complex contains three- and two- coordinate lead(II) atoms linked by μ 2 -bridging oxygen atoms, whilst in the chloride complex four- and two-coordinate metal atoms are also associated by μ 2 -bridging oxygen atoms. In [Pb 2 Br 6 ](FI 3 Dea) 2 the nearest coordination environment of metal atoms consists of bromine atoms only, while the H 3 Dea + cations are not coordinated to lead atoms at all. The structural differences between the coordination environments of the lead atoms are discussed in connection with the inert pair effect. All compounds possess ionic type crystal structures.

Open Access June 2, 2014

Neue metallorganisch substituierte Zinn-Tellur-Verbindungen. Synthese und Kristallstrukturen von [{Cp(CO)₂Fe}₄Sn₂Te₂], [{Cp(CO)₃Mo}₄Sn₂Te₂] und [{Cp(CO)₃Mo}₄Sn₄Te₆] / New Organometallic Tin-Tellurium Compounds. Syntheses and Crystal Structures of [{Cp(CO)₂Fe}₄Sn₂Te₂], [{Cp(CO)₃Mo}₄Sn₂Te₂] and [{Cp(CO)₃Mo}₄Sn₄Te₆]

Kurt Merzweiler, Harald Kraus

Page range: 621-626

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Abstract

Organometallic tin halides R 2 SnCl 2 (R = {Cp(CO) 2 Fe}, {Cp(CO) 3 Mo}) react with Te(SiMe 3 ) 2 to form the compounds [{Cp(CO) 2 Fe} 4 Sn 2 Te 2 ] 1, [{Cp(CO) 3 Mo} 4 Sn 2 Te 2 ] 2 and [{Cp(CO) 3 Mo) 4 Sn 4 Te 6 ] 3. According to crystal structure determinations, 1 and 2 contain planar Sn 2 Te 2 rings. 3 consists of an adamantane-like Sn 4 Te 6 framework.

Open Access June 2, 2014

Darstellung und Struktur dreier verschiedener Bis(ethylendiamin)-kupfer(II)-tetraborate / Preparation and Structure of Three Different Bis(ethylenediamine) Copper(II) Tetraborates

Mahmood Shakibaie-Moghadam, Ulrich Timper, Gert Heller

Page range: 627-634

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Abstract

Three different bis(ethylenediamine) Copper(II) tetraborates have been prepared: Cu(en) 2 [B 4 O 5 (OH) 4 ] · 2B(OH) 3 (A), 2{Cu(en) 2 B(OH) 3 · H 2 O[B 4 O 5 (OH) 4 ]} · H 2 O (B) and {Cu(H 2 O) 2 [B 4 O 5 (OH) 4 ] 2 }(μ-H 2 O){Ag(en) 2 } · (μ-H 2 O){Na(H 2 O) 2 ) (C). The crystal structure analyses of A (monoclinic, P2 1 /c, a = 1282.5(1), b = 1020.8(1), c = 1510.5(2) pm; β = 96.66(1)°, Z = 4), B (monoclinic, Pc, a = 1254.4(1), b = 914.1(1), c = 1594.2(2) pm; β = 94.79(1)°, Z = 2) and C (triclinic, P1, a = 846.3(3), b = 917.9(3), c = 928.1(7) pm; α = 93.71(6)°, β = 104.79(3)°, γ = 103.23(2)°; Z = 1) show that all compounds contain the tetraborate ion [B 4 O 5 (OH) 4 ] 2- . In A and B, there are tetraborate ions and boric acid molecules. The coordination sphere of the Cu 2+ ion is Jahn-Teller distorted, coordinated by 2 en groups with 4 Cu-N distances between 196 and 206 pm, as well as by 2 OH groups with Cu-O distances of 251 to 274 pm. In C, the Cu 2+ ion is surrounded by 6 OH groups, and the Ag + ion by 2 en and 2μ-H 2 O molecules.

Open Access June 2, 2014

Crystal Structure of Sr_0.2Ca_2.8Tl₂O₆

Kirsten Ruck, Horst Borrmann, Arndt Simon

Page range: 635-636

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Abstract

The crystal structure of Sr 0.2 Ca 2.8 Tl 2 O 6 has been determined by single crystal X-ray diffraction. The compound crystallizes in space group Pbam (No. 55) with a = 11.228(1), b = 16.471(1) and c = 3.3326(3) Å. It is isostructural with Ca 3 In 2 O 6 and SrCa 2 In 2 O 6 .

Open Access June 2, 2014

Das Anion [R₂Al-AlR₂Br]^- (R = CH(SiMe₃)₂) mit Aluminium-Aluminium- und terminaler Aluminium-Brom-Bindung / The Anion [R₂Al-AlR₂Br]^- (R = CH(SiMe₃)₂) with an Aluminium -Aluminium and a Terminal Aluminium -Bromine Bond

Werner Uhl, Uwe Schütz, Siegfried Pohl, Wolfgang Saak

Page range: 637-641

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Abstract

Tetrakis[bis(trimethylsilyl)methyl]dialane(4) (1) with an Al-Al bond reacts with LiBr in n-pentane in the presence of chelating N.N.N'.N'-tetramethylethylenediamine (TMEDA) to yield the monobromo adduct [Li(TMEDA) 2 ] + [R 2 Al-AlR 2 Br] - 4. Compound 4 is unstable in ethereal solution and decomposes with quantitative formation of LiBr and the starting compound 1. Crystal structure determination of 4 C 5 H 10 shows a terminal Al-Br bond in an anion with a four-coordinated aluminium atom neighbouring a three-coordinated, coordinatively unsaturated aluminium atom. While the Al-Al bond length is not significantly different (264.3 pm) as compared to the data for 1, the Al-Br bond is rather long (247.6 pm) indicating a weak coordinative bonding.

Open Access June 2, 2014

Gold(I) Complexes of Organic Nitrogen Compounds: Synthesis and Structures of (Phthalimido)(triphenylphosphine)gold(I) in Crystals C₆H₄(CO)₂N(AuPPh₃) and C₆H₄(CO)₂N( AuPPh₃) · CHCl₃

Peter Lange, Annette Schier, Jürgen Riede, Hubert Schmidbaur

Page range: 642-646

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Abstract

[O(AuPPh 3 ) 3 ] + BF 4 - has been found to be a powerful aurating reagent for phthalimide, to give (phthalimido)(triphenylphosphine)gold(I) (1) in high yield. Two different crystal systems, with or without CHC1 3 molecules in the unit cell, have been obtained. In both cases the monoaurated diacylamido complex C 6 H 4 (CO) 2 N(AuPPh 3 ) (1) is present as a monomer with linear two-coordinate gold atoms. The N-Au(I) bond lengths (2.028(4), 2.040(4) Å) are similar to those found in other monoaurated complexes of the type R ] R 2 N(AuPPh 3 ) with strongly electron-withdrawing organic substituents R 1 , R 2 . Crystal data: 1, monoclinic, P2 1 /c, a = 9.948(1), b = 15.712(1), c = 14.651(1) Å, β = 103.40(1)°, V = 2227.7 Å 3 , Z = 4; 1·CHCl 3 , orthorhombic, P2 1 2 1 2 1 , a = 8.889(1), b = 10.349(1), c = 29.198(2) Å, V = 2686.0 Å 3 , Z = 4.

Open Access June 2, 2014

A New Synthesis of Dimethylgold(III) Chloride Using Tetramethyltin

Martin Paul, Hubert Schmidbaur

Page range: 647-649

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Abstract

The reaction of HAuCl 4 or AuCl 3 with Sn(CH 3 ) 4 in methanol at low temperatures gives [(CH 3 ) 2 AuCl] 2 in yields from 40 to 45%.

Open Access June 2, 2014

Die Kristallstrukturen von Li[PF₆] und Li[AsF₆]: Zur Kristallchemie von Verbindungen A[E^VF₆] / The Crystal Structures of Li[PF₆] and Li[AsF₆]: On the Crystal Chemistry of Compounds A[E^VF₆]

Caroline Röhr, Rüdiger Kniep

Page range: 650-654

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Abstract

Li[PF 6 ] (rhombohedral, R3̅; a = 493.2(2), c = 1265.8(4) pm; Z = 3) and Li[AsF 6 ] (rhombohedral, R3̅; a = 501.6(1), c = 1302.8(4) pm; Z = 3) are isotypes of the Li[BiF 6 ] structure. The E v -elements P(As) as well as lithium are in a nearly perfect octahedral coordination by fluorine. The crystal structures of the fluoro-compounds A[E V F 6 ] (A = Li, Na, K, Rb, Cs; E v = P, As, Sb, Bi) can be divided in two groups: i. with A and E v in a NaCl like arrangement and ii. with A and E v in a CsCl like arrangement. The coordination numbers (CN) of the A-sites (CN between 6 and 12) depend on the ratio of radii r(E V5+ )/r(A + ).

Open Access June 2, 2014

Darstellung und Kristallstruktur der Cäsium-Selenidogermanate(IV) Cs₄Ge₄Se₁₀ · 2CH₃OH und Cs₄Ge₂Se₈ / Preparation and Crystal Structure of the Cesium Selenidogerm anates(IV) Cs₄Ge₄Se₁₀ · 2CH₃OH and Cs₄Ge₂Se₈

W. S. Sheldrick, B. Schaaf

Page range: 655-659

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Abstract

Methanolothermal reaction of Cs 2 CO 3 with Ge and Se at 190 °C yields Cs 4 Ge 4 Se 10 · 2 CH 3 OH and Cs 4 Ge 2 Se 8 , the structures of which have been determined by X-ray structural analysis. The anion [Ge 4 Se 10 ] 4 in Cs 4 Ge 4 Se 10 )·2 CH 3 OH displays an adamantane-like structure in which four GeSe 4 tetrahedra are linked via joint vertices. In contrast Cs 4 Ge 2 Se 8 contains the novel dinuclear anion [Ge 2 Se 8 ] 4- , the first example of a selenidogermanate(IV) exhibiting Se 2 bridging units. Two GeSe 4 tetrahedra are linked in this anion through Se-Se bonds to yield a six-membered ring, which displays a chair conformation and crystallographic C 2h symmetry.

Open Access June 2, 2014

Übergangsmetallkomplexe mit Schwefelliganden, CI. Synthese und Struktur von N₂H₅[Fe(N₂H₄)(S₂C₆H₄)₂] · 1,33N₂H₄ / Transition Metal Complexes with Sulfur Ligands, Cl. Synthesis and Structure of N₂H₅[Fe(N₂H₄)(S₂C₆H₄)₂] · 1,33N₂H₄

Dieter Sellmann, Helge Friedrich, Falk Knoch

Page range: 660-664

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Abstract

Attempts to coordinate N 2 H 4 to [Fe(S 2 C 6 H 4 ) 2 ] fragments lead to N 2 H 5 [Fe(N 2 H 4 )(S 2 C 6 H 4 )2], which crystallizes from MeOH/N 2 H 4 solutions as the solvate [(N 2 H 5 ){Fe(N 2 H 4 )(S 2 C 6 H 4 ) 2 } · 1,33 N 2 H 4 ]. 1, and has been characterized by X-ray structure analysis. 1 contains three discrete N 2 H 5 + cations, four N 2 H 4 solvate molecules and three independent [Fe(N 2 H 4 )(S 2 C 6 H 4 ) 2 ] - anions which are connected via an extended network of N-H ··· N and N-H ··· S bridges. N 2 H 5 [Fe(N 2 H 4 )(S 2 C h H 4 ) 2 ] and 1 contain high-spin Fe(III) centers and labile N 2 H 4 ligands.

Open Access June 2, 2014

Synthesis and Characterization of Cu(II) and Mono-and Dinuclear Pb(II) Complexes Derived from 3,5-Diacetyl-1,2,4-triazole

P. Souza, A. I. Matesanz, A. Arquero, V. Fernandez

Page range: 665-671

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Abstract

Template 1:1 condensation of 3,5-diacetyl-1,2,4-triazole with thiocarbohydrazide or car- bohydrazide in the presence of 1 equivalent of Pb(SCN) 2 produces mononuclear [2 + 1] complexes 1 and 3. The analogous reaction with thiosemicarbazide and semicarbazide produces the dinuclear [1+2] complex 2 and the mononuclear metal free 4. The carbohydrazide derivative 3 reacts with the carbohydrazide or the 1,3-diaminopropane to yield the macrocyclic dinuclear complexes 5 and 6. Direct reaction of 3,5-diacetyl-1,2,4-triazole with thiocarbohydrazide. carbohydrazide, thiosemicarbazide and semicarbazide leads to open [1+1] ligands L 1 , L 2 , L 3 , L 4 , and closed [1+1] ligands (mesocyclic ligands) L 5 and L 6 were prepared by addition of 1 equivalent of LiOH to the reaction mixture. The reaction of open and mesocyclic [1+1] ligands with copper(II) salts gives [CuLX 2 ] and [Cu 2+ L 2- ] complexes. All these compounds have been characterized by 1 H NMR, IR, electronic and mass spectra and by analytical data.

Open Access June 2, 2014

Unexpected Formation of 1-Amino-4,4,5,5-tetramethyl-3- (5,5,6,6-tetramethyl-1,4,5,6-tetrahydropyridazin-3-yl)pyrrolidin-2-one

Jürgen Voss, Rüdiger Röske, Gunadi Adiwidjaja

Page range: 672-674

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Abstract

The title compound 3 is formed on reaction of octamethyldispiro[2.1.2.1]octane-4,8-dione (1) with hydrazine. Its structure is established by X -ray diffraction analysis.

Open Access June 2, 2014

Tris(1,10-phenanthroIine)iron(II) Complexes. Influence of 4,7-Donor Substitution on the Redox Potential [1]

Michael Levis, Ulrich Lüning, Michael Müller, Michael Schmittel, Clemens Wöhrle

Page range: 675-682

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Abstract

Several new 4.7-donor substituted 1.10-phenanthrolines were synthesized and the corresponding tris(1,10-phenanthroline)iron(II) complexes were studied by cyclic voltammetry. All iron(II) complexes showed fully reversible waves at scan rates between 50 and 500 mV/s. For some redox systems the kinetics in their reaction with chlorine was studied. Complexes 7k and 71 significantly extent the potential range of tris(1,10-phenanthroline)iron(II) complexes.

Open Access June 2, 2014

A Pentamethylcyclopentadienyl Ligand Functionalized with a Pendant Pyridyl Group; Crystal Structure of its Ferrocene-Type Iron Complex

Ulrich Siemeling, Beate Neumann, Hans-Georg Stammler

Page range: 683-686

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Abstract

The novel cyclopentadiene HMe 4 C 5 CH 2 CMe 2 py [py = 2-(4-tert-butyl)pyridyl] 2H has been prepared from tetramethylfulvene and lithiated 2-isopropyl-4-tert-butylpyridine. Lithiation of 2H with Bu n Li and subsequent reaction with FeCl 2 yields the ferrocene (2) 2 Fe, which crystallizes in the triclinic space group P1̅ with a = 8.368(1), b = 8.468(1), c = 14.313(1) Å, α = 80.64(1), β = 86.67(1), γ = 80.12(1)° and V = 985.4(2) Å 3 .

Open Access June 2, 2014

Synthesis of Novel 3-Acetyl-2-hydroxy-1-N,N-diacetylaminocarbazole Derivatives

M. Sekar, S. Vanitha, K. J. Rajendra Prasad

Page range: 687-690

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Abstract

The synthesis of hitherto unknown 3-acetyl-2-hydroxy-1-N,N-diacetylaminocarbazole (3a-f), is reported. The hydroxyiminocarbazoles (2a-f), prepared from 1-oxo-1,2,3,4-tetra-hydrocarbazoles (1a -f) on treatment with acetyl chloride in acetic anhydride yielded the title compounds (3a-f).

Open Access June 2, 2014

Neue Synthesen für homonukleare Cobalthydrid-Clusterverbindungen / New Synthetic Routes to Homonuclear Cobalt Hydride Clusters

Jörg J. Schneider

Page range: 691-696

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Abstract

Several homonuclear cobalt hydride clusters are accessible by reacting the complexes (η 5 -Cp R )Co(η 2 -ethene) 2 (R = H 5, Me 5 ) 3, 4 with (C 2 H 5 ) 2 AlH followed by alcoholysis of the crude reaction mixtures. Depending on the degree of alkyl substitution, different nuclearities of the resulting clusters have been observed. In the case of the pentamethyl substituted derivative (η 5 -Cp*)Co(η 2 -ethene) 4 a mixture of di-, tri- and tetranuclear cobalt hydride clusters namely [(η 5 -Cp*)Co] 2 H 3 1, [(η 5 -Cp*)Co] 3 H 4 2 and [(η 5 -Cp*)Co] 4 H 4 7 were formed and separated by repeated crystallization. When reacting the parent compound (η 5 -Cp)Co(η 2 -ethene) 3 with (C 2 H 5 ) 2 AlH and quenching the reaction mixture with alcohol at low temperature, the tetranuclear cobalt cluster [(η 5 -Cp)Co] 4 H 4 5 is the main product. Aside from this, trace amounts of the cobalt alkylidine cluster [(η 5 -Cp)Co] 4 μ-[C(CH 3 )]H 6 were formed as detected by mass spectrometry. For the first time a direct synthesis of [(η 5 -Cp**)Co] 3 H 4 10 and [(η 5 -Cp**)Co] 4 H 4 11 was achieved by reaction of cobalt atoms with tetramethyl-ethyl-1,3-cyclopentadiene (mixture of isomers) in methylcyclohexane at -120 °C. However, the main product of this metal atom reaction is the mononuclear cobalt sandwich compound (η 5 -Cp**)Co(η 4 -tetramethyl-ethyl-1,3-cyclopentadiene) 9 as a mixture of isomers. The trinuclear cobalt alkylidine cluster [(η 5 -Cp*)Co] 3 μ 3 -[C(CH 3 )] 2 8 is formed when reacting (η 5 -Cp R )Co(η 2 -ethene) 2 3 with equimolar amounts of di-isobutyl-aluminium- hydride or the borabicyclus 9-BBN.

Open Access June 2, 2014

Covalent Adducts from 2-Substituted 5-Arylazotropones and Nucleophiles and their Fate

Marino Cavazza, Francesco Pietra

Page range: 697-701

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Abstract

Working in (CD 3 ) 2 SO/MeOH 98:2, 2-methoxy-5-[(4-methylphenyl)azo]-2,4,6-cyclohepta- trien-1-one (1a) was found to add either MeO - , giving the stablegcw-dimethoxy α-adduct 2a, or EtS - , to give initially to the C-2 α-adduct 4 a; on neutralization, the latter gave ipso (C-2) replacement of OMe by SEt, while the former returned to the starting material, via the neutral α-adduct 3a. In contrast, in the same medium, 2-ethylthio-5-[(4-methylphenyl)azo]-2,4,6-cy- cloheptatrien-1-one (5 a) was found to add EtS - at both C-2 and C-7; on neutralization products of both ipso substitution (5 a) and ipso- plus tele-substitution (C-7) (8) were isolated.

Open Access June 2, 2014

Festphasensynthese von Muramyldipeptidderivaten und Untersuchung ihrer biologischen Aktivität / Solid Phase Synthesis of Muramyl Dipeptide Derivatives and Investigations on their Biological Activities

Jochen Tschakert, Wolfgang Voelter

Page range: 702-716

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Abstract

New muramyl dipeptide derivatives with exchanged carbohydrate residues are described. Each derivative is synthesized via a solid phase synthesis using an aminomethyl anchor resin. All synthetic products can be isolated in good yields. Their biological activities are tested by the luminol-dependent chemiluminescence associated with the phagocytosis of opsonized zymosan by granulocytes.

Open Access June 2, 2014

Synthesis and Spectroscopic Study of Pentacarbonyl(η²-tetracyanoethylene) Metal(0) Complexes of the Group 6 B Elements

İzzet A. Mour, Saim Özkar

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Abstract

Pentacarbonyl(η 2 -tetracyanoethylene) metal(0) complexes of chromium, molybdenum and tungsten have been synthesized by the photochemical reaction of hexacarbonyl metal(o) with tetra- cyanoethylene in toluene at room temperature. The complexes were purified by chromatography and recrystallization, and characterized by UV- visible, IR and 13 C NMR spectroscopy. Tetra- cyanoethylene is symmetrically bonded to the M(CO) 5 unit through its carbon-carbon double bond as an η 2 -ligand. The spectral data are discussed in terms of the metal → ligand π interaction.

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

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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 49 Issue 5

Issue of Zeitschrift für Naturforschung B

Zur Kristallchemie der Oxoplatinate. Eine neue Phase der Zusammensetzung Sr4-ϰNaϰPtO6 (ϰ = 0,33) / On the Crystal Chemistry of Oxoplatinates. A New Phase of the Composition Sr4-ϰNaϰPtO6 (ϰ = 0,33)

Abstract

Ein Beitrag zur Kristallchemie der oxidischen Alkali-Erdalkali-Edelmetall-Perowskite. Synthese und Kristallstruktur von NaBa4Cu0,5Pt1,5O8 / A Contribution to the Crystal Chemistry of Alcaline Alealine Earth Precious Metal Perovskites. Synthesis and Crystal Structure of NaBa4Cu0,5Pt1,5O8

Abstract

Das erste Oxocuprat/-Arsenat mit Kupfer in gemischter Valenz: Cu(Mg2,56Cu0,44)Cu(AsO4)3 / The First Oxocuprate/Arsenate Containing Mixed Valent Copper:Cu(Mg2,56Cu0,44)Cu(AsO4)3

Abstract

Abstract

μ2-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh4[X(N-Iodsuccinimid)2] · CH3CN mit X = Cl, Br, / μ2-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh4[X(N-Iodosuccinimide)2] · CH3CN with X = Cl, Br, I

Abstract

Benzyliden-und Methylen-bis-silyltriflate als neue Synthesebausteine für Organosiliciumpolymere/ Benzylidene-and Methylene-bis-silyltriflates as New Synthetic Materials for Organosilicon Polymers

Abstract

Crystal Structure of Lead(II) Complexes with 2,2'-Iminodiethanol

Abstract

Abstract

Darstellung und Struktur dreier verschiedener Bis(ethylendiamin)-kupfer(II)-tetraborate / Preparation and Structure of Three Different Bis(ethylenediamine) Copper(II) Tetraborates

Abstract

Crystal Structure of Sr0.2Ca2.8Tl2O6

Abstract

Das Anion [R2Al-AlR2Br]- (R = CH(SiMe3)2) mit Aluminium-Aluminium- und terminaler Aluminium-Brom-Bindung / The Anion [R2Al-AlR2Br]- (R = CH(SiMe3)2) with an Aluminium -Aluminium and a Terminal Aluminium -Bromine Bond

Abstract

Gold(I) Complexes of Organic Nitrogen Compounds: Synthesis and Structures of (Phthalimido)(triphenylphosphine)gold(I) in Crystals C6H4(CO)2N(AuPPh3) and C6H4(CO)2N( AuPPh3) · CHCl3

Abstract

A New Synthesis of Dimethylgold(III) Chloride Using Tetramethyltin

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Die Kristallstrukturen von Li[PF6] und Li[AsF6]: Zur Kristallchemie von Verbindungen A[EVF6] / The Crystal Structures of Li[PF6] and Li[AsF6]: On the Crystal Chemistry of Compounds A[EVF6]

Abstract

Darstellung und Kristallstruktur der Cäsium-Selenidogermanate(IV) Cs4Ge4Se10 · 2CH3OH und Cs4Ge2Se8 / Preparation and Crystal Structure of the Cesium Selenidogerm anates(IV) Cs4Ge4Se10 · 2CH3OH and Cs4Ge2Se8

Abstract

Übergangsmetallkomplexe mit Schwefelliganden, CI*. Synthese und Struktur von N2H5[Fe(N2H4)(S2C6H4)2] · 1,33N2H4 / Transition Metal Complexes with Sulfur Ligands, Cl*. Synthesis and Structure of N2H5[Fe(N2H4)(S2C6H4)2] · 1,33N2H4

Abstract

Synthesis and Characterization of Cu(II) and Mono-and Dinuclear Pb(II) Complexes Derived from 3,5-Diacetyl-1,2,4-triazole

Abstract

Unexpected Formation of 1-Amino-4,4,5,5-tetramethyl-3- (5,5,6,6-tetramethyl-1,4,5,6-tetrahydropyridazin-3-yl)pyrrolidin-2-one

Abstract

Tris(1,10-phenanthroIine)iron(II) Complexes. Influence of 4,7-Donor Substitution on the Redox Potential [1]

Abstract

A Pentamethylcyclopentadienyl Ligand Functionalized with a Pendant Pyridyl Group; Crystal Structure of its Ferrocene-Type Iron Complex

Abstract

Synthesis of Novel 3-Acetyl-2-hydroxy-1-N,N-diacetylaminocarbazole Derivatives

Abstract

Neue Synthesen für homonukleare Cobalthydrid-Clusterverbindungen / New Synthetic Routes to Homonuclear Cobalt Hydride Clusters

Abstract

Covalent Adducts from 2-Substituted 5-Arylazotropones and Nucleophiles and their Fate

Abstract

Festphasensynthese von Muramyldipeptidderivaten und Untersuchung ihrer biologischen Aktivität / Solid Phase Synthesis of Muramyl Dipeptide Derivatives and Investigations on their Biological Activities

Abstract

Synthesis and Spectroscopic Study of Pentacarbonyl(η2-tetracyanoethylene) Metal(0) Complexes of the Group 6 B Elements

Abstract

Zur Kristallchemie der Oxoplatinate. Eine neue Phase der Zusammensetzung Sr_4-ϰNa_ϰPtO₆ (ϰ = 0,33) / On the Crystal Chemistry of Oxoplatinates. A New Phase of the Composition Sr_4-ϰNa_ϰPtO₆ (ϰ = 0,33)

Ein Beitrag zur Kristallchemie der oxidischen Alkali-Erdalkali-Edelmetall-Perowskite. Synthese und Kristallstruktur von NaBa₄Cu_0,5Pt_1,5O₈ / A Contribution to the Crystal Chemistry of Alcaline Alealine Earth Precious Metal Perovskites. Synthesis and Crystal Structure of NaBa₄Cu_0,5Pt_1,5O₈

Das erste Oxocuprat/-Arsenat mit Kupfer in gemischter Valenz: Cu(Mg_2,56Cu_0,44)Cu(AsO₄)₃ / The First Oxocuprate/Arsenate Containing Mixed Valent Copper:Cu(Mg_2,56Cu_0,44)Cu(AsO₄)₃

μ₂-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh₄[X(N-Iodsuccinimid)₂] · CH₃CN mit X = Cl, Br, / μ₂-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh₄[X(N-Iodosuccinimide)₂] · CH₃CN with X = Cl, Br, I

Crystal Structure of Sr_0.2Ca_2.8Tl₂O₆

Das Anion [R₂Al-AlR₂Br]^- (R = CH(SiMe₃)₂) mit Aluminium-Aluminium- und terminaler Aluminium-Brom-Bindung / The Anion [R₂Al-AlR₂Br]^- (R = CH(SiMe₃)₂) with an Aluminium -Aluminium and a Terminal Aluminium -Bromine Bond

Gold(I) Complexes of Organic Nitrogen Compounds: Synthesis and Structures of (Phthalimido)(triphenylphosphine)gold(I) in Crystals C₆H₄(CO)₂N(AuPPh₃) and C₆H₄(CO)₂N( AuPPh₃) · CHCl₃

Die Kristallstrukturen von Li[PF₆] und Li[AsF₆]: Zur Kristallchemie von Verbindungen A[E^VF₆] / The Crystal Structures of Li[PF₆] and Li[AsF₆]: On the Crystal Chemistry of Compounds A[E^VF₆]

Darstellung und Kristallstruktur der Cäsium-Selenidogermanate(IV) Cs₄Ge₄Se₁₀ · 2CH₃OH und Cs₄Ge₂Se₈ / Preparation and Crystal Structure of the Cesium Selenidogerm anates(IV) Cs₄Ge₄Se₁₀ · 2CH₃OH and Cs₄Ge₂Se₈

Übergangsmetallkomplexe mit Schwefelliganden, CI. Synthese und Struktur von N₂H₅[Fe(N₂H₄)(S₂C₆H₄)₂] · 1,33N₂H₄ / Transition Metal Complexes with Sulfur Ligands, Cl. Synthesis and Structure of N₂H₅[Fe(N₂H₄)(S₂C₆H₄)₂] · 1,33N₂H₄

Synthesis and Spectroscopic Study of Pentacarbonyl(η²-tetracyanoethylene) Metal(0) Complexes of the Group 6 B Elements