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1989 (280)
81Author    Gertrud Kräuter, Frank Weller, Kurt DehnickeRequires cookie*
 Title    Synthesen und Kristallstrukturen der Kronenether-Komplexe [Li3(12-Krone-4)30 2CCH3] [Cd(Se4)2], {[K(18-Krone-6)]2[Hg(Se4)2]}2 und [Na(15-Krone-5)]N03 Syntheses and Crystal Structures of the Crown Ether Complexes [Li3(1 2 -Crown-4 )3 0 :CCH3][Cd(Se4):], {[K(18-Crown-6)]2[Hg(Se4)2]}2< and [Na(15-Crown-5)]N03  
 Abstract    Crown Ether C om plexes o f Lithium. Sodium , and Potassium. Synthesis. Crystal Structure [Li3(12-crow n-4)30 2C C H 3][C d(Se4)2] has been prepared by the reaction of [Li(12-crown-4)]2Se6 with Cd(CKCCH?) in ethanolic solution. The corresponding polyselenide com plex o f mercury is formed by"the reaction o f [K(18-crown-6)]2Se(l with H g (0 2CCH 3)2 in the same solvent. Both com pounds form dark red crystals, which were characterized by single crystal X-ray structure determ inations. The only product to be isolated from the reaction o f B i(N 0 3)3-5 H 20 with [Na(15-crown-5)]2Se6 in ethanolic solution was [Na(15-crow n-5)]N 03, whose structure has also been determ ined. [Li3(12-crown-4)30 2C C H 3][C d(Se4)2]: space group Pbca, Z = 8. 1404 observed independent reflexions. R = 0.097. Lattice dim ensions (19 °C): a — 1981.5(6). b — 1400.3(1), c — 3268.9(9) pm. The com pound forms a dicationic ensem ble, in which three lithium ions coordinate with the oxygen atom s o f the acetate ion. In the anions the cadmium atom is coordinated tetrahedrally by four selenium atoms o f two Se42 units. {[K (18-crow n-6)]2[H g(Se4)2]}2: space group P1.Z = 1. 3210 observed independent reflexions, r = 0.055. Lattice dim ensions (19 °C): a = 1057.4(2). b = 1130.6(2), c = 2000.1(2) pm. a = 88.52(1)°, ß = 85.86(1)°, y = 66.22(1)°. The com pound has a com plex ionic structure, in which the formula units form centrosym m etric dimers through K —O contacts between two cations. In addition there are K-Se contacts with the spiro-bicyclic anions, which -together with 6 K -O bonds within the crowns — lead to the coordination number o f 8 for the remaining potassium ions. [N a(15-crow n -5)]N 03: space group P 2 ,2 ,2 ,. Z = 4. 1211 observed independent reflexions. R = 0.052. Lattice dim ensions (20 °C): a = 912.9(2). b = 989.6(1). c = 1658.3(3) pm. The com pound forms ion pairs, in which the sodium atom coordinates with the five oxygen atoms oi the crown ether, as well as with two oxygen atoms o f the nitrate ion with Na— O bond lengths o f 240 and 247 pm. 
  Reference    Z. Naturforsch. 44b, 444 (1989); eingegangen am 21. N ovem ber 1988/24. Januar 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0444 
 Volume    44 
82Author    EckehardV. Dehmlow, Andreas WinterfeldtRequires cookie*
 Title    New Cyclopentadienones from Sterically Demanding Inner Acetylenes and Dicobalt-octacarbonyl  
 Abstract    A lkyne-C arbon Monoxide R eaction, M etal Carbonyl Catalysis, Cyclopentadienones, Cycloalkanocyclopentadienones Acetylenes carrying one bulky substituent can be transform ed into symmetrically or asym m etri­ cally substituted cyclopentadienones 2 or 3 when they are heated with Co2(C O)s and carbon monoxide. Intram olecular cyclizations yielding compounds 5 are also possible. 
  Reference    Z. Naturforsch. 44b, 455—458 (1989); received D ecem ber 5 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0455 
 Volume    44 
83Author    Jingtang Chen, Thomas Pili, Wolfgang BeckRequires cookie*
 Title    Metallkomplexe mit biologisch wichtigen Liganden, L [1] Palladium(II)-, Platin(II)-und Kupfer(II)-Komplexe von a-Aminosäure-N-Glykosiden und von Fructose-Aminosäuren (Amadori-Verbindungen) Metal Complexes of Biologically Important Ligands, L [1] Palladium(II), Platinum(II) and Copper(II) Complexes of a-Amino Acid-N-Glycosides and of Fructose-Amino Acids (Amadori-Compounds)  
 Abstract    Amino Acid-N-Glycosides, N -(l-D eoxy-D -fructos-l-yl)-am ino Acids, Palladium (II), Platinum (II), C opper(II) Complexes Various N-glycosides derived from glucose and a-am ino acids and the isomeric Amadori com­ pounds form bis(chelate) complexes of copper(II), palladium (II) and platinum (II). The IR spectra indicate that the ligands are coordinated through the amino group and a carboxylate oxygen atom. 
  Reference    Z. Naturforsch. 44b, 459 (1989); eingegangen am 24. November 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0459 
 Volume    44 
84Author    Xv Polysulfonylamines, Armand Blaschette, Karin Linoh, Dietrich Koch, Ludger ErnstRequires cookie*
 Title    Polysulfonylamine, XV [1] Synthese von N-bernsteinsäurediamid zu y-DimesyIamino-zl^y-butenolid Succinic Diamide to y-Dimesylamino-zl/1:'-butenolide  
 Abstract    N .N .N 'N '-Tetram esyl Dicarboxylic D iamides, Silver Dimesylam ide. Dicarboxylic Dichlorides, y-Dimesylamino-J^ '-butenolide, a-A ngelicalactone N .N .N '.N '-T etram esyl dicarboxylic diamides Ms2N C (0) — Q —C (0)N M s; [Q = (C H 2)" with n = 0 (2a), 2 (2b), 3 (2c), 4 (2d); Q = o-phenylene (2e)] were prepared by reacting AgNM s2 (1) with the appropriate dicarboxylic dichlorides in acetonitrile at room tem perature (2a, 2 c —2e) or at 0 °C (2b), respectively. Under similar conditions, malonic dichloride undergoes an elimination, forming AgCl, HNM s2 and probably polymeric C , 0 2. A t 20 °C in C H 3CN, the succinic acid derivative 2b eliminates one mole of HNM s2 and, by ring closure, yields y-dimesylamino-Zl^:-butenolide (4a), the first example of a stable y-am ino-zP'-butenolide. T reatm ent of 4a with aqueous NaOH results in the form ation of NaNM s2 and sodium succinate. Crystalline 4a is thermally stable at 100 °C; no signs of an isomerization 4a —> y-dimesylamino-zT^-butenolide could be detected. Unlike the structurally related a-angelicalactone (4c), whose brom ination affords the saturated dibrom olactone 9 as a mixture of cis-and m w s-isom ers, 4a adds bromine (20 °C, CHC1,) under ring cleavage to form B rC (0)C H 2C H B rC (0)N M s2 (7). The new com­ pounds 2, 4a and 7 as well as the stereoisom ers of 9 were characterized by spectroscopic ('H and l3C NM R. MS, IR) and analytical m ethods. In order to obtain reference values for the chemical shifts of 7, the following new compounds were prepared: C H 3(C H :)2C (0)N M s2 (10c, from 1 and butvryl chloride); C H ,C H ^C H B rC (0)N M si (12c, from 1 and 2-bromobutyryl brom ide); C 2H 50 C (0) C H 2C H B rC (0)N M s2 (13, from 7 with ethanol and from 4a by simultaneous reaction with brom ine and ethanol). 
  Reference    Z. Naturforsch. 44b, 465 (1989); eingegangen am 28. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0465 
 Volume    44 
85Author    UlrichH W Hildebrand, Johann LexRequires cookie*
 Title    Untersuchungen zur Struktur von Co(III)-und Ni(II)-Komplexen der Pyridin-2,6-di(monothiocarbonsäure) Structural Investigations of Co(III)-and Ni(II)-Complexes of Pyridine-2,6 -di(monothiocarboxylic Acid)  
 Abstract    Pyridine-2,6-di(monothiocarboxylic Acid) Complexes The preparation and structure elucidation of C o(III)-and Ni(II)-complexes of pyridine-2, 6-di(monothiocarboxylic acid) are reported. The Co ion chelates two of these tridentate ligands to form the octahedral bis(pyridine-2,6-dicarbothioato)-cobaltat(III). whereas the Ni ion coordi­ nates only with two of the three binding sites of each ligand to give a tetrahedral complex. B is(pyridine-2,6-dicarbothioato)-nickelat(II) is stable only in the absence of 0 2; it polymerizes by formation of disulfid bridges between the free thiocarboxyl groups if exposed to air. 
  Reference    Z. Naturforsch. 44b, 475 (1989); eingegangen am 7. N ovember 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0475 
 Volume    44 
86Author    Thomas Kaukorat, Reinhard SchmutzlerRequires cookie*
 Title    Uber intramolekulare Donator-Akzeptor-Wechselwirkungen in N,N'-Dimethylharnstoff-Derivaten des Phosphors Intramolecular Donor-Acceptor Interactions in N,N'-Dimethylurea Derivatives of Phosphorus  
 Abstract    D on or-A ccep tor Interactions, N .N '-D im ethylurea. Spirophosphoranes The reaction of [M e:NCH 2CH ;N (M e)P C l]*C r 1 with N .N '-dim ethyl-N .N '-bis(trim 
  Reference    Z. Naturforsch. 44b, 481 (1989); eingegangen am 1. Septem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0481 
 Volume    44 
87Author    Mohamed Fathy, AbdelrazekRequires cookie*
 Title    Heterocyclic Synthesis with Nitriles: A Novel Synthesis of Some Thiophene and Thieno[2,3-d]pyrimidine Derivatives, II [1]  
 Abstract    /3-Thiocyanatomethyl Cinnam onitrile, Thiophene D erivatives, Thieno[2.3-d]pyrim idine D erivatives 
  Reference    Z. Naturforsch. 44b, 488—492 (1989); received May 31/O ctober 17 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0488 
 Volume    44 
88Author    Andreas Frankenau, Kurt DehnickeRequires cookie*
 Title    Synthesis and IR Spectrum of [MoC14(NC1)] 2  
 Abstract    N -C hloro-N itrene-M olybdenum Tetrachloride, Synthesis, IR Spectra 
  Reference    Z. Naturforsch. 44b, 493 (1989); eingegangen am 1. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0493_n 
 Volume    44 
89Author    Wolfgang Hiller, Eva Hartmann, Kurt DehnickeRequires cookie*
 Title    Synthesis and Crystal Structure of the Cyclic Hydrazido Complex {Fe2Cl4[(NSiMe3)(CPh)]2N2}  
 Abstract    Cyclic Hydrazido Complex {F e2Cl4[(N SiM e3)(C P h)]2N 2} , Synthesis, IR Spectrum, Crystal Structure 
  Reference    Z. Naturforsch. 44b, 495 (1989); eingegangen am 5. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0495_n 
 Volume    44 
90Author    Klaus-Jürgen Range, Manfred WildenauerRequires cookie*
 Title    A gN b30 8-II, eine Hochdruckphase mit neuartiger Tunnelstruktur AgNb30 8-II, a High-Pressure Phase with a Novel Tunnel Structure  
 Abstract    High-Pressure M odification. Crystal Structure A quenchable high-pressure phase o f A g N b ,0 8 (A gN b 30 8-II) could be synthesized at 35 kbar. 1100 °C in a m odified Belt-type apparatus. The structure (Ibam , a = 7.343, b = 10.415. c = 
  Reference    Z. Naturforsch. 44b, 499 (1989); eingegangen am 9. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0499_n 
 Volume    44 
91Author    Jung Su, Han, Werner WolfsbergerRequires cookie*
 Title    Darstellung und Charakterisierung von einigen unsymmetrischen Chlordiorganophosphanen RR'PCI Preparation and Characterization of Some Unsymmetrical Chlorodiorganophosphines RR'PCI  
 Abstract    Chlorodiorganophosphines. NM R Spectra Som e unsymmetrical chlorophosphines RR'PCI were prepared by the reaction o f RPC1: (R = CH., C;H5. /-C3 H7 , C6 H5) with Grignard reagents R'M gCl (R' = c-C5 Hy, c-C6 H n , /-C3 H7) and charac­ terized by elem ental analyses and spectroscopic data (IR . 3IP and l3C NM R). 
  Reference    Z. Naturforsch. 44b, 502 (1989); eingegangen am 20. Januar 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0502_n 
 Volume    44 
92Author    Wolfgang Blase, Gerhard Cordier, Rüdiger Kniep, Roswitha SchmidtRequires cookie*
 Title    Phasenbeziehungen im System Naln—Sn und die Kristallstrukturen der intermediären Verbindungen NaInSn2 und NaInSn4 Phase Relations in the System Naln —Sn and the Crystal Structures of the Intermediate Compounds NaInSn2 and NaInSn4  
 Abstract    The quasibinary system N aln —Sn contains the intermediate phases Na9In9Sn, Na9In9Sn2, N alnSn, N a2In2Sn3, NaInSn2 and NaInSn4. With the exception o f N a2In2Sn3 (stable only between 134 °C and 365 °C), crystals o f the ternary com pounds were grown from the melt and were 
  Reference    Z. Naturforsch. 44b, 505 (1989); eingegangen am 16. Januar 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0505 
 Volume    44 
93Author    Olefine, Christian Bessenbacher, Wolfgang KaimRequires cookie*
 Title    Elektronenreiche Cyclically Conjugated tt Electrons and 3 Neighbouring N Electron Pairs  
 Abstract    Bildung des ersten N,N-persilylierten 1,4-Diaminoethens über eine 1.2.3-Triazolin(4)-Zwischenstufe mit 8 cyclisch konjugierten ^-Elektronen und 3 benachbarten N-EIektronenpaaren Electron Rich Olefins, 3 Formation of the First N.N'-Persilvlated 1,4-Diaminoethene via a 1.2.3-Triazoline(4)-Intermediate with 8 Organosilicon Com pounds, H eterocycles, M olecular C onform ation. PE Spectra. ESR Spectra Exhaustive reductive silylation o f 2-trim ethylsilyl-1,2,3-triazole (1) using M e,SiC l/K yields the new E -l.l,4,4-tetrakis(trim ethylsilyl)-l,4-d iazab utene(2) (4) as final product together with N (S iM e3)v Initial reductive 1,4-addition to 1 leads to formation o f 1,2,3-tris(trim ethylsilyl)-1.2.3-triazolin e(4) (2) as an intermediate which is rapidly reduced and silylated further to give the butene 4. Partial j z overlap within the five-m em bered ring 2 containing 8 . t electrons and three neighbouring unshared electron pairs is evident from NM R shifts and electron transfer reaction with T C N E . Photoelectron spectroscopy of 4 and the lability o f its radical cation 4+' as studied by E SR show that this system cannot adopt a planar conformation in contrast to the tetrazene(2) analogue. 
  Reference    Z. Naturforsch. 44b, 511 (1989); eingegangen am 20. Septem ber/28. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0511 
 Volume    44 
94Author    Hans-Jürgen Meyer, Joachim PickardtRequires cookie*
 Title    Die Kristallstrukturen von Strontium-und Bariumhexacyanoferrat(III)-Hexamethylentetramin-Hydraten Strukturmodell für Additionsverbindungen der Alkali-und Erdalkalimetallhexacyanoferrate mit Hexamethylentetramin The Crystal Structures of Hydrates of Strontium and Barium Hexacyanoferrate(III) with Hexamethylenetetramine Structural Model for Adducts of the Hexacyanoferrates of Alkaline and Alkaline Earth Metals with Hexamethylenetetramine  
 Abstract    Crystal Structure. H exacyanoferrate(III), H exam ethylenetetram ine By reaction o f m ethanolic solutions o f hexam ethylenetetram ine with aqueous solutions of hexacyanoferrates(III) of strontium and barium resp., crystals o f the com pounds were obtained. 
  Reference    Z. Naturforsch. 44b, 519 (1989); eingegangen am 19. Februar/22. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0519 
 Volume    44 
95Author    Ralf Steudel, Thomas Göbel, Gabriele HoldtRequires cookie*
 Title    The Molecular Nature of the Hydrophilic Sulfur Prepared from Aqueous Sulfide and Sulfite (Selmi Sulfur Sol) [1]  
 Abstract    Sulfur Sol. Polythionates. Elem ental Sulfur. W ackenroder Reaction Hydrophilic sulfur sols prepared by reaction o f aqueous sulfide and sulfite at low pH have been studied by chem ical analysis, ion-pair chrom atography, and reversed-phase HPLC. The approxi­ mate com position of the sol is x (N a H S 0 4/N a;S 0 4) • vS" • zN a2S,"Oh with n = 6 —10 and m = 4 —16. The elem ental sulfur S" accounts for 17% and the polythionate sulfur for 10% o f the dry weight (sulfate: 18%). On aging of the sol at 20 °C the long-chain polythionates decom pose to elem ental sulfur and tetrathionate as well as pentathionate. The higher chemical reactivity of this sol compared to Sx is explained by the fact that 45% o f the zero oxidation state sulfur (S°) are present as non-S8 m olecules. 
  Reference    Z. Naturforsch. 44b, 526 (1989); received January 20. 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0526 
 Volume    44 
96Author    Dieter Fenske, PaulG. MauéRequires cookie*
 Title    Zur  
 Abstract    Reaktion von [iy5-CpMCl4] (M = Nb, Ta) mit E(SiMe3)2 (E = S, Se) Die Kristallstrukturen von [Cp8Ta6S10][TaSCl5], [Cp3Ta3S7Cl2], [Cp4Ta4Si3] und [Cp3Nb3Se5Cl2] Reaction of [?75-CpMCl4] (M = Nb, Ta) with E(SiMe3) 2 (E = S, Se) The Crystal Structures of [Cp8Ta6S10][TaSCl5], [Cp3Ta3S7Cl2], [Cp4Ta4S13] and [Cp3Nb3Se5Cl2] X -R ay, Crystal Structure, M ixed V alence N b —Se C om plexes, C yclopentadienyl C om plexes [?75-CpMCl4] (M = N b, Ta) reacts with E (SiM e3)2 (E = S, Se) to form different multinuclear clusters. The cation [Cp8Ta6S10]2+ (1) consists o f a planar Ta2S2-ring o f which each Ta is coordi­ nated to two Cp2TaS2-fragments. [Cp4Ta4S 13] (3) can be derived from [Cp3Ta3S7Cl2] (2) by addi­ tion o f a CpTaS6-unit to a triangle of Ta-atom s bridged by S-and S2-ligands. The niobium atoms in [Cp3N b3Se5Cl2] (4) arrange in a chain structure with Nb coordination numbers varying from 4 —6. 
  Reference    Z. Naturforsch. 44b, 531 (1989); eingegangen am 1. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0531 
 Volume    44 
97Author    Guogang Liang, NicolasA. Corfù, Helmut SigelRequires cookie*
 Title    Influence of Decreasing Solvent Polarity (Dioxane-Water Mixtures) on the Stability of Metal Ion Complexes Formed with Phosphate Monoesters  
 Abstract    The acidity constants o f H (R —M P)~, where R —M P: = 4-nitrophenyl phosphate (N PhP2). phenyl phosphate (PhP2) and D -ribose 5'-m onophosphate (R ibM P2). and the stability constants of the binary C u (R -M P) com plexes w'ere determ ined by potentiom etric pH titrations in aqueous solution and in 20. 30, 40 and 50% (v/v) dioxane-water mixtures. The solvent influence on the corresponding equilibrium constants is com pared with the same influence on previously studied systems containing uridine 5'-triphosphate. formate or acetate. The influence o f the solvent com position on the various ligand (L) system s was evaluated by constructing log Km(L) versus pK[j(L) plots; in all cases straight lines are obtained with slopes close to 1. This indicates that in all these system s, despite the different negative charges o f the involved ligands, the solvent effect on proton binding and on metal ion binding is approxim ately o f the same size: A decreasing solvent polarity resulting from the addition o f increasing am ounts o f organic solvent to the aqueous solutions favors the affinity o f the negatively charged ligands for protons and metal ions as well. Information o f this type is considered important because the 'effective' or 'equivalent solution' dielectric constants in active-site cavities o f enzym es are reduced com pared with the dielectric constant o f bulk water; i. e., in protein cavities also a decreased 'solvent polarity' is occurring and this is expected to affect the stability o f metal ion-ligand bonds. 
  Reference    Z. Naturforsch. 44b, 538 (1989); received N ovem ber 28 1988 
  Published    1989 
  Keywords    Phosphate M onoester, Metal Ion C om plexes, Solvent Influence, Stability Constants, A ctive-Site Cavities o f Enzymes 
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 Identifier    ZNB-1989-44b-0538 
 Volume    44 
98Author    H. Erbert, W. Roesky, UweO. Tten, Regine Herbst, Mathias NoltemeyerRequires cookie*
 Title    Preparation and Structures of a,/?-U nsaturated Aliphatic Diazenes  
 Abstract    Crystal Structure. Conjugated m m s-D iazenes, Unsymm etrical A zines, 1.3-D ithiolanes 
  Reference    Z. Naturforsch. 44b, 543 (1989); eingegangen am 23. D ezem ber 1988 
  Published    1989 
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 Identifier    ZNB-1989-44b-0543 
 Volume    44 
99Author    FrankW. Eller, Fritjof Schmock, Kurt DehnickeRequires cookie*
 Title    Synthesis and Crystal Structure of 2-Trimethylsilyl-l,3-bis-trimethylsilylimino- 1,3-dihydro-isoindole and the Crystal Structure of Hexakis(trimethylsilyl)-1,4-benzdiamidine  
 Abstract    2-Trim ethylsilyl-l,3-bis-trim ethylsilylim ino-1.3-dihydro-isoindole, H exakis(trim ethylsilyl)-1.4-benzdiam idine, Synthesis, Crystal Structure 
  Reference    Z. Naturforsch. 44b, 548 (1989); eingegangen am 18. Januar 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0548 
 Volume    44 
100Author    Th Fetzer, A. Lentz, T. D. Ebaerdem AekerRequires cookie*
 Title    Einkristallzüchtung und Röntgenstrukturanalyse polymerer l:l-Komplexe von CuBr2 und CuCl2 mit Pyrazin aus Gelen Crystal Growth in Gels and X-Ray Characterization of Polymerie 1:1-Complexes of C uB r2 and CuCl2 with Pyrazine  
 Abstract    Pyrazine, Copper C om plexes, Polymerie C om plexes. G el Crystallization Single crystals o f Cu(pz)Br2 and C u(pz)C l2 were grown by using gel m ethods with tetram ethoxysilane as the gel-forming reagent. Thermal decom position is interpreted. Crystal data for the bromo complex: monoclinic, space group C2/m with a — 1239.2(3) pm , b = 685.9(2) pm, c = 390.7(3) pm, ß — 96,23(5)°. Crystal data for the chloro-com plex: m onoclinic, space group C2/m with a = 1197.1(3) pm. b = 684.9(3) pm . c = 370.1(3) pm. ß = 95.96(5)°. Crystal structure analyses reveal that CuHal2 m olecules are bonded by pyrazine to form linear chains. These chains are cross-linked by bridging halogen atom s. 
  Reference    Z. Naturforsch. 44b, 553 (1989); eingegangen am 26. Januar 1989 
  Published    1989 
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 Identifier    ZNB-1989-44b-0553 
 Volume    44 
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