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1982[X]
1Author    Barbara Balbach, Reinhold Alt, ManfredL. ZieglerRequires cookie*
 Title    Structural Investigations on Four-Membered Ring Systems, III* Crystal and Molecular Structures of frattS-2,4-Bis(trimethylsilyl)-2,4-dihydro-l,3-dithietane- 1.1.3.3-tetroxide, 2,2,4,4-Tetramethyl-3-pyrrolidinocyclobutanone and 2.2.4.4-Tetramethyl-l-phenyl-3-pyrrolidinocyclobutanol  
 Abstract    The molecular structures of the title compounds have been determined by X-ray methods. In the bis(trimethylsilyl) substituted dithietane the (CH3)3Si groups are in trans position; the C2S2-ring is planar. In the cyclobutanone the pyrrolidine group occupies an equatorial position, as does the phenyl group in the cyclobutanol. In the latter the hydroxyl group is trans to the pyrrolidine ring. The four-membered carbon rings are folded. 
  Reference    Z. Naturforsch. 37b, 1005—1013 (1982); eingegangen am 6. April 1982 
  Published    1982 
  Keywords    X-ray, Cyclobutanol, Dithietanetetroxide 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1005.pdf 
 Identifier    ZNB-1982-37b-1005 
 Volume    37 
2Author    Werner Kruppa, Dieter Bläser, Roland Boese, Günter SchmidRequires cookie*
 Title    Heteronucleare Clustersysteme, XX [1] ^3-Bi8mutio-cyclo-tris(tricarbonyliridium) (3 Ir-Ir), BiIr3(CO)9 Darstellung und Strukturuntersuehung eines neuartigen Iridiumclusters Heteronuclear Cluster Systems, XX [1] iM3-Bismutio-cyclo-tris(tricarbonyliridium)(3Ir-Ir), BiIr3(C0)g - Synthesis and Structural Investigation of a Novel Iridium Cluster  
 Abstract    The synthesis of BiIr3(CO)9 is described. IR and mass spectroscopic data are discussed. The structure of BiIr3(CO)9 was solved by X-ray analysis. The structural data are discussed and compared with those of the related compounds Ir4(CO)i2 and Bi[Co(CO)4]3, respec-tively. 
  Reference    Z. Naturforsch. 37b, 209—213 (1982); eingegangen am 29. September 1981 
  Published    1982 
  Keywords    Iridium Cluster, Bismuth Cluster, Synthesis, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0209.pdf 
 Identifier    ZNB-1982-37b-0209 
 Volume    37 
3Author    Werner Winter, AntonThomas Butters, Rieker, Yasuo ButsuganRequires cookie*
 Title    Synthesis and Structure of l,2-Bis(2,4,6-tri-fert-butylphenyl)ethane  
 Abstract    The title compound 9, C38H62, was prepared by dehalogenation of 2,4,6-tri-£er£-butyl-benzyl chloride (7a). It crystallizes in the monoclinic space group C2/c with Z = 4. a = 10.923(7), b = 17.910(3), c = 17.395(3) A and ß = 91.87(3)° (the cell constants refer to 173 K). The structure was solved by direct methods and refined by full-matrix least squares to 7? = 0.073 for all 3853 reflexions (|Fo| > 0). On account of steric repulsions, the central ethane bond, which lies on a twofold crystallographic axis, is stretched to 1.567(4) A. Close packing of the molecules in layers parallel the ac-plane leads to boat-deformations of the benzene rings. Room-temperature data sets of weakly diffracting crystals [a = 10.948(0), b= 17.97(1), c= 17.52(2) and ß = 91.9(1)°] do not give rise to an artificial shortening of the central ethane bond of 9. Evidently, poor data quality or lack of resolution have not to be considered as an explanation for the unusual short ethane bond [1.47(3) A] in the first undamped hexaphenylethane [Stein, Winter, and Rieker (1978)]. Historical Background 
  Reference    Z. Naturforsch. 37b, 855—862 (1982); received March 15 1982 
  Published    1982 
  Keywords    X-ray, Steric Hindrance, Hindered Ethanes 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0855.pdf 
 Identifier    ZNB-1982-37b-0855 
 Volume    37 
4Author    Gabriela WeberRequires cookie*
 Title    A 1:1 Host-Guest Complex between ('18-crown-6') and m-Nitroaniline: Mere Stoicheiometry or a Genuine 1:1 Adduct ?  
 Abstract    The stoicheiometrically 1:1 adduct of 1,4,7,10,13,16-hexaoxa-cyclooctadecane with m-nitroaniline, C18H30N2O8, Mr = 402.45, crystallises from toluene in red-orange prisms, (probable) space group Pi, a = 801.8(3), b = 920.4(3), c = 1403.3(4) pm, a = 80.40(4), ß = 79.79(4), y = 85.95(3)°, V = 1.07910 nm 3 , Z = 2, dcaic. = 1.238 Mgm~ 3 . Structure refinement converged at R = 0.060 (Rw = 0.002) for 2915 diffractometer data. 
  Reference    Z. Naturforsch. 37b, 1250—1254 (1982); received March 22 1982 
  Published    1982 
  Keywords    Crown Ether, m-Nitroaniline, H Bridges, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1250.pdf 
 Identifier    ZNB-1982-37b-1250 
 Volume    37 
5Author    Paul Rustemeyer, ErnstOtto Fischer, Klaus Ackermann, Ulrich SchubertRequires cookie*
 Title    (CO)13Re3COSi(C6H5)3, ein neuartiger Typ eines metallorganischen Acyl-Komplexes mit dreibindigem Sauerstoff A New Type of an Organometallic Acyl Complex with a Three-Coordinate Oxygen Atom  
  Reference    Z. Naturforsch. 37b, 1279—1283 (1982); eingegangen am 17. Mai 1982 
  Published    1982 
  Keywords    /; 2 -Acyl Complex, Bridging Oxygen Atom, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1279.pdf 
 Identifier    ZNB-1982-37b-1279 
 Volume    37 
6Author    Joachim Pickardt, Norbert RautenbergRequires cookie*
 Title    Die Kristallstruktur von Hexa- The Crystal Structure of Hexa-^-chloro-/^- oxo-tetrakis [hexamethylenetetraminecopper- (II)], [Cu4Cl60(C6H12Nl)4], a Copper(II) Complex with a Structure Related to that of Beryllium Oxoacetate  
 Abstract    -tetrakis [hexamethy lentetramin -kupfer(II)], [CU4C160(C6H12N4)4], einem Kupfer(II)-Komplex mit Berylliumoxoace-tat-ähnlicher Struktur By reaction of solutions of CuCl2 • 2H20 and hexamethylenetetramine, C6H12N4, in acetone, a complex [Cu4Cl60(C6Hi2N4)] could be ob-tained as single crystals. An X-ray analysis shows that the complex has a structure related to that of basic beryllium acetate. An oxygen atom is tetrahedrally surrounded by four cop-per atoms which, together with six chlorine atoms, form an adamantane-like core. Each copper atom is bonded via a nitrogen atom to a hexamethylenetetramine molecule. 
  Reference    Z. Naturforsch. 37b, 1355—1357 (1982); eingegangen am 28. Juni 1982 
  Published    1982 
  Keywords    Copper(II) Complexes, Chloro Complexes, Hexamethylenetetramine, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1355_n.pdf 
 Identifier    ZNB-1982-37b-1355_n 
 Volume    37 
7Author    Beatrix Milewski-Mahrla, Hubert SchmidbaurRequires cookie*
 Title    Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates  
 Abstract    Reactions of pentamethylantimony (CH^sSb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramethylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed. The crystal structures of the hydrogen-dibenzoate (1), hydrogen-ortho-phthalate (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter-actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH^Sb-tetrahedron in 1 is distorted by two benzoate oxygen atoms (at 304(2) and 340(2) pm). The cation in 2 is largely undistorted and the anion has a bydrogenpbthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate. 
  Reference    Z. Naturforsch. 37b, 1393—1401 (1982); eingegangen am 5. Juli 1982 
  Published    1982 
  Keywords    Pentamethylantimony, Tetramethylstibonium Salts, Hydrogendicarboxylates, Hydrogen Bonding, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1393.pdf 
 Identifier    ZNB-1982-37b-1393 
 Volume    37 
8Author    Alfred Gieren, Michail KokkinidisRequires cookie*
 Title    Structure Investigations o f Agonists o f the Natural Neurotransmitter Acetylcholine II [1| X-ray Structure Analysis o f Trimethyl(4-oxopentyl)ammonium-chloride  
 Abstract    The crystal structure of Trimethyl(4-oxopentyl)ammonium-chloride ([(C H 3) 3 N —(CH^aCOCHjJCl-) (1) was determined by an X-ray structure analysis. 1 crystallizes in the orthorhombic space group P21 21 21 with a = 10.440 (3), b = 14.600 (9), c = 6.804 (9) A and with four formula units per unit cell. The structure was solved by a Patterson and a successive Fourier synthesis. The least squares refinement yielded an R-value o f 0.064 for 1077 observed reflections. The cation o f 1 is derived from acetylcholine by replacement o f the ester oxygen with a CH2 group. It shows a potent nicotinic activity and a significant difference in conformation as compared with acetylcholine. In the crystal structure the anions are oriented stereospecifically with respect to the tetrahedron of the quaternary ammonium group. The geometry o f two triangles formed by the quaternary nitrogen atom, the oxygen atom o f the carbonyl group, and by either o f the two anions nearest to the quaternary ammonium group is characteristic for the nicotinic activity o f 1. 
  Reference    Z. Naturforsch. 37c, 282 (1982); received December 231981 
  Published    1982 
  Keywords    X-ray, Neurotransmitter, Cation-Anion Interactions, Structure-Activity Relationships 
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 TEI-XML for    default:Reihe_C/37/ZNC-1982-37c-0282.pdf 
 Identifier    ZNC-1982-37c-0282 
 Volume    37 
9Author    Beate Meyer, Hartmut WunderlichRequires cookie*
 Title    Kristallstrukturen von zwei Modifikationen des Mo(IV)-Komplexsalzes [(Et2PS2)3Mo3S(S2)3] (Et2PS2)- Crystal Structures of Two Modifications of the Mo(IV) Complex Salt [(Et2PS2)3M03S(S2)3] + (Et2PS2)  
 Abstract    Tris(diethyldithiophosphinato)-tris-/<-disulfido-^3-thiotriangulo-trimolybd©num(IV)-di-ethyldithiophosphinate, [(et2PS2)3Mo3S(S2)3] + (et2PS2) _ , crystallizes in two orthorhombic modifications with crystallographic parameters of A: a = 20.651(3), 6=10.152(2), c = 19.019(2) A, Pca2x, Z = 4 and B: a = 20.128(2), 6= 15.655(2), c = 12.608(1) A, Puma, Z = 4. Both crystal structures were determined from 2886 (A) and 3414 (B) X-ray data with R factors of 0.058 and 0.045, respectively. The Mo atoms form a trinuclear Mo3S(S2)3 cluster with local symmetry close to C3V in both modifications which differ in the packing of anions and cations and in the conformation of the ethyl groups. The av. distance Mo-Mo is 2.737 A, the coordination number of the Mo atoms is 7 within the cluster and 9 on inclusion of the S atoms of the dithiophosphinato group. 
  Reference    Z. Naturforsch. 37b, 1437—1441 (1982); eingegangen am 24. Mai 1982 
  Published    1982 
  Keywords    Trinuclear Molybdenum Cluster, Dithiophosphinato Complexes, Crystal Structure, X-ray 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1437.pdf 
 Identifier    ZNB-1982-37b-1437 
 Volume    37 
10Author    R. Tacke, A. Bentlage, W. S. Sheldrick, L. Ernst, K. StoepelRequires cookie*
 Title    Sila-Pharmaka, 24. Mitt. [1] Sila-Analoga von Nifedipin-ähnlichen 4-Aryl-2.6-cümethyl-1.4-dihydropyridin- 3.5-dicarbonsäure-dialkylestern, II Sila-Drugs, 24 th Communication [1] Sila-Analogues of Nifedipine-Like Di alkyl 4-Aryl-2,6-dimethyl-l,4-dihydropyridine- 3,5-dicarboxylates, II  
 Abstract    In the course of systematic studies on sila-substituted drugs the nifedipine-like 1.4-di-hydropyridine derivatives 4 a, 4 b and 4 c were prepared and investigated with respect to sila-substitution effects. By X-ray diffraction analyses 4 a, 4 b and 4 c were found to be isostructural. The C/Si-analogues exhibit similar spasmolytic activities (in vitro, guinea pig ileum), comparable with that of nifedipine. However, the compounds differ sub-stantially in their in vivo activity, as measured by the antihypertensive effect on the renal-hypertensive rat. The experimental results are discussed with respect to the carbon/silicon exchange. 
  Reference    Z. Naturforsch. 37b, 443—450 (1982); eingegangen am 25. September 1981 
  Published    1982 
  Keywords    Sila-Analogues of Nifedipine Derivatives, X-ray, Pharmacological Activity, Structure-Activity Relationships 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0443.pdf 
 Identifier    ZNB-1982-37b-0443 
 Volume    37 
11Author    Horst Elias, Elke Hilms, Helmut PaulusRequires cookie*
 Title    X-Ray Structures and Spectral Properties of 4-Coordinate Copper(II) and Palladium(II) Complexes with a Tridentate ONN-Schiff Base Ligand  
 Abstract    The tridentate mono-basic Schiff base N-(2-diethylaminoethyl)salicylaldimine =Hsal-en-NEt2 forms complexes 1 = [(sal-en-NEt2)MY] with divalent metals M (Y = halide). The preparation of three copper(II) complexes la (Y = Br), lb (Y = Cl), and lc (Y = SCN) and one palladium(II) complex 1(1 (Y = Cl) is described and the UV/VIS spectra of these complexes in methanol and chloroform are compared and discussed. The crystals of la • CHCI3, lb • CHCI3, and Id • CHCI3 are all isotypic and crystallize in the ortho-rhombic space group Pbca, whereas the solvent-free crystals of 1 b (and also 1 a) are monoclinic with the space group P2i/c. The metal is 4-coordinate with an almost planar ONNY donor atom arrangement around the palladium and with a distorted arrangement around the copper. The crystals consist of separate non-bridged complex units and the chloroform is not coordinated. 
  Reference    Z. Naturforsch. 37b, 1266—1273 (1982); received March 31 1982 
  Published    1982 
  Keywords    X-ray, UV/VIS Spectra, Tridentate ONN Schiff Base, Copper(II) Complexes, Palladium(II) Complexes 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1266.pdf 
 Identifier    ZNB-1982-37b-1266 
 Volume    37 
12Author    Reinhold Tacke, Haryanto Linoh, MoayadT. Attar-Bashi, WilliamS. Sheldrick, Ludger Ernst, Roland Niedner, Joachim FrohneckeRequires cookie*
 Title    Sila-Pharmaka, 26. Mitt. [1] Darstellung und Eigenschaften potentiell curarewirksamer Silicium-Verbindungen, III Sila-Pharmaca, 26th Communication [1] Preparation and Properties of Silicon Compounds with Potential Curare-Like Activity, III  
 Abstract    The potentially curare-hke silicon compounds 8a-Sf were synthesized and investigated with respect to their structure-activity relationships. The conformations of the com-pounds in the solid state and in solution were studied by X-ray diffraction analysis (8a-8e) and *H NMR spectroscopy (8a-8f), respectively. The muscle relaxing properties of 8a-8f were investigated on the mouse. The observed structure-activity relationships are not in accordance with the classical "14 A model" for neuromuscular blocking agents. Einführung 
  Reference    Z. Naturforsch. 37b, 1461—1471 (1982); eingegangen am 19. April 1982 
  Published    1982 
  Keywords    Silicon Compounds, Curare-Like Activity, X-ray, Conformational Analyses, Structure-Activity Relationships 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-1461.pdf 
 Identifier    ZNB-1982-37b-1461 
 Volume    37