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1982[X]
21Author    Joachim Pickardt, Norbert RautenbergRequires cookie*
 Title    Metallkomplexe mit Hexamethylentetramin als Ligand, VI [1] Kristallstruktur von Bis-hexamethylentetramin-bisisocyanatokupfer(II), [CU(NCO)2(C6H12N4)2]  
 Abstract    Crystals of the complex [Cu(NCO)2(C6Hi2N4)2] could be obtained by reaction of copper-(Il)nitrate, hexamethylenetetramine, and KNCO in CHCI3 as a solvent. The crystals are triclinic, space group Cl, Z = 4, a = 1373.1(9), b = 2083.1(9), c = 642.6(3) pm, a = 91.05(4), ß = 90.54(6), y = 107.39(6)°. The copper atom is bonded to two terminal cyanato groups via the nitrogen atoms, and to two liexamethylentetramine molecules. In the solid state the coordination of the copper atom is, however, tetragonal pyramidal, because there is an additional, rather long bond to one of the hexamethylenetetramine molecules of the neighbouring complex unit, resulting in the formation of chains. 
  Reference    Z. Naturforsch. 37b, 1569—1572 (1982); eingegangen am 6. September 1982 
  Published    1982 
  Keywords    Cupric Complexes, Isocyanato Complexes, Hexamethylenetetramine, Crystal Structure 
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 Identifier    ZNB-1982-37b-1569 
 Volume    37 
22Author    H. Holler, W. Kurtz, D. Babel, Sonderforschungsbereich, (. Kristallstruktur, Chemische Bindung, W. KnopRequires cookie*
 Title    Die Kristall-und magnetische Struktur von BaCrF5 Crystal and Magnetic Structure of BaCrF5  
 Abstract    A single crystal X-ray structure analysis of orthorhombic BaCrFs (a — 1393.8(1), b = 571,1(1), c = 494,7(1) pm), which crystallizes in the structure type of BaGaF5, space group P2i2i2i, yielded Cr-F distances in the range of 187.3 to 194.9 pm, average 190.2 pm. Using powder neutron diffraction data taken at 2.2 K a G-type antiferromagnetic structure with spin alignment along the c direction of the lattice was worked out. Single crystal susceptibility data were consistent with this model and in addition showed a small net moment, probably due to spin canting, to be present below the Neel temperature of TN = 3.4 K. The orientation of this moment along the b axis is in accordance with the space group symmetry as well, chemical and magnetic cell being the same. From powder susceptibility data an exchange energy of —3.74 K (g = 2.02) was obtained by fitting Fisher's model. The low bridging angle of Cr-F-Cr = 137.4° within the eis corner-sharing chain of octahedra is made responsible for the weak antiferromagnetism in BaCrFs, which is compared to that of other chromium(III) fluorides. 
  Reference    (Z. Naturforsch. 37b, 54—60 [1982]; eingegangen am 21. August 1981) 
  Published    1982 
  Keywords    Pentafluorochromate(HI), Crystal Structure, Magnetic Structure, Magnetic Susceptibility 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0054.pdf 
 Identifier    ZNB-1982-37b-0054 
 Volume    37 
23Author    Doris Bodenstein, Axel Brehm, PeterG. Jones, Einhard Schwarzmann, GeorgeM. SheldrickRequires cookie*
 Title    Darstellung und Kristallstruktur von Arsen(III)phosplior(V)oxid, AsP04 Preparation and Crystal Structure of Arsenic(III) Phosphorus(V) Oxide, AsP04  
 Abstract    The compound ASPO4 was prepared from AS2O3 and P2O5 in a sealed tube at 673 K. The crystal structure, isostructural with As02, was refined to R = 0.021 [Pnma, a — 843.15(10), b = 502.29(10), c = 720.39(12) pm, Z = 4]. The structure consists of infinite layers. The arsenic(III) atoms are coordinated by three oxygen atoms at right angles; phosphorus(V) by four oxygens in the form of a distorted tetrahedron. 
  Reference    Z. Naturforsch. 37b, 136—137 (1982); eingegangen am 7. Oktober 1981 
  Published    1982 
  Keywords    Sealed-tube Synthesis, Crystal Structure, Arsenic(III), Phosphorus(V) 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0136.pdf 
 Identifier    ZNB-1982-37b-0136 
 Volume    37 
24Author    Ulrich Müller, Hans-Dieter DörnerRequires cookie*
 Title    Eine neue Synthese, das Schwingungsspektrum und die Kristallstruktur von Tetraphenylarsonium-hydrogendichlorid As(C6H5)4 [C12H] A New Synthesis, the Vibrational Spectrum and the Crystal Structure of Tetraphenylarsonium Hydrogendichloride AsfCeHsMC^H]  
 Abstract    As(C6H 5)4 + [Cl2H]-crystallizes in the monoclinic space group B2/b with four formula units per unit cell, the lattice constants being a— 1704, 6= 1751, c — 705 pm and y = 92.73°. The crystal structure was determined and refined from X-ray diffraction data to a residual index of R = 0.043. The CI2H-ion is situated on an inversion center with a C1---C1 distance of 309 pm. The IR and Raman spectra confirm the presence of sym-metrical CI2H -ions; the observed splitting of IR bands can be explained by factor group analysis. A simple procedure for the preparation consists of the reaction of HCl with As(C6H 5)4Cl. 
  Reference    Z. Naturforsch. 37b, 198—200 (1982); eingegangen am 1. Oktober 1981 
  Published    1982 
  Keywords    Tetraphenylarsonium Hydrogendichloride, Synthesis, Crystal Structure, Raman Spectra, IR Spectra 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0198.pdf 
 Identifier    ZNB-1982-37b-0198 
 Volume    37 
25Author    Frank Kübel, Joachim Strähle+Requires cookie*
 Title    Polymere Dimethyl-und Diphenylglyoximatokomplexe des Cobalts und Eisens mit 4.4' -Bipyridin als Brückenligand. Die Kristallstruktur des Bis(dimethylglyoximato)4.4'-bipyridincobalt(II)* Polymeric Dimethyl-and Diphenylglyoximato Complexes of Cobalt and Iron with 4,4'-Bipyridine as a Bridging Ligand. The Crystal Structure of Bis(dimethylglyoximato)4,4'-bipyridine Cobalt(II)  
 Abstract    Polymeric bis(dimethyl-and diphenylglyoximato)-complexes of Fe(II) and Co(II) with 4,4'-bipyridine as a bridging ligand have been synthesized from the glyoximato metal complexes and 4,4'-bipyridine in ethanol. The Co(II) compounds are paramagnetic and surprisingly stable against oxidation. The iron complexes are weak electrical conductors with approximately 10 -9 ß -1 cm _1 . Bis(dimethylglyoximato)-4,4'-bipyridine cobalt(II) crystallizes triclinic in the space group PT with Z — 1. The crystal structure is built up by linear chains of alternating Co(II) glyoximato complexes and axial bonded 4,4'-bipyridine bridges. The compound is characterized by strong Co-N-bonds of 189 pm within the glyoximato moiety and weak bonds of 228 pm to the bipyridine ligand. The two hetero-cycles of the bipyridine are coplanar, therefore the local symmetry of the complex is D 2 
  Reference    Z. Naturforsch. 37b, 272—275 (1982); eingegangen am 23. Oktober 1981 
  Published    1982 
  Keywords    Iron and Cobalt Glyoximato-4, 4'-Bipyridine Complexes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0272.pdf 
 Identifier    ZNB-1982-37b-0272 
 Volume    37 
26Author    Doris Bodenstein, Axel Brehm, PeterG. Jones, Einhard Schwarzmann, GeorgeM. SheldrickRequires cookie*
 Title    Darstellung und Kristallstruktur von Arsen(III)phosphor(V)oxidhydroxid As2P05(0H) Preparation and Crystal Structure of the Arsenic(III) Phosphorus(V) Oxide Hydroxide As2POs(OH)  
 Abstract    The title compound was prepared by heating the hydrolysis products of ASPO4 in a sealed tube. The crystal structure was determined and refined to R = 0.028 [P2i/n, a = 454.5(1), b = 1229.0(2), c = 972.8(3) pm, ß = 100.13(2)°, Z = 4]. The structure, which is not isostructural with As30s(0H), consists of infinite layers, containing pyramidal AS(III)03 and tetrahedral P(V)04 groups, and stabilised by hydrogen bonding of the form P-O-H -O-P. 
  Reference    Z. Naturforsch. 37b, 531—533 (1982); eingegangen am 24. November 1981 
  Published    1982 
  Keywords    Sealed Tube Synthesis, Crystal Structure, Arsenic(III), Phosphorus(V) 
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 Identifier    ZNB-1982-37b-0531 
 Volume    37 
27Author    Karl-Friedrich Tebbe, Bernhard FreckmannRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, V [1]  
 Abstract    Darstellung und Kristallstruktur des Tetrammin-palladium(II)-oktaiodids, [Pd(NH3)4]I8 Studies on the Polyhalides, V [1] Preparation and Crystal Structure of [Pd(NH3)4]l8 The new compound [Pd(NH3)4]l8 crystallizes monoclinically in the space group P2i/m with a = 959.0 pm, b = 835.4 pm, c = 1301.1 pm, ß = 103.37° and Z = 2 formula units. The crystal structure has been solved by 'direct methods' and refined to R = 0.057 with 1357 observed reflections. The structure consists of quadratically coordinated cations [Pd(NH3)4] 2+ and planar, Z-shaped and completely ordered octaiodide anions I8 2 ~. According to the sequence of interatomic distances d(I-I) = 295.0 pm, 289.9 pm, 336.2 pm, 279.1 pm, 327.0 pm, 339.3 pm, 273.8 pm the anions may be described as [I3- • I2 • (I~ • I2)]-The iodide-iodine sides (I- • I2) are joined with the distance d(I---I) = 364.1 pm to a slightly bent triiodide chain being part of an octaiodide ribbon ^ [Is 2-]-Next contact spacings between neigh-boring anions start at d(I---I) = 403.7 pm. 
  Reference    Z. Naturforsch. 37b, 542—549 (1982); eingegangen am 26. November 1981 
  Published    1982 
  Keywords    Palladium Complex, Polyhalide, Octaiodide Ion, Iodine Chain, Crystal Structure 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0542.pdf 
 Identifier    ZNB-1982-37b-0542 
 Volume    37 
28Author    Josef Hahn, Marianne Baudler, Carl Krüger, Yi-Hung TsayRequires cookie*
 Title    Beiträge zur Chemie des Phosphors, 116 [1] Kernresonanzspektren und Kristallstruktur von Tri -tert-butyl -cy clotriphosphan Contributions to the Chemistry of Phosphorus, 116 [1] NMR Spectra and Crystal Structure of Tri-terf-butylcyclotriphosphane  
  Reference    Z. Naturforsch. 37b, 797—805 (1982); eingegangen am 1. März 1982 
  Published    1982 
  Keywords    Tri-ier^-butylcyclotriphosphane, Threo-Membered Ring Compounds, NMR Spectra, Crystal Structure 
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 Identifier    ZNB-1982-37b-0797 
 Volume    37 
29Author    Kristall, Achim Müller, Hartmut Bögge, Erich Krickemeyer, Gerald Henkel, Bernt KrebsRequires cookie*
 Title    Isopoly-und Heteropoly-Thioanionen  
 Abstract    -und Molekülstrukturen von (PPh4)2[(WS4)WS(WS4)], CS2[(WS4)W0(WS4)H20] 2 H20 und (AsPh4)2[(WS4)Ni(WS4)] Isopoly-and Heteropoly-Thioanions. Crystal and Molecular Structures of (PPh 4)2[(WS4)WS(WS4)]. Cs2[(WS4)W0(WS4)H20] • 2 H20 and (AsPh4)2[(WS4)Ni(WS4)] The crystal and molecular structures of (PPh4)2[(WS4)WS(WS4)] (LA) and CS2[(WS4)W0(WS4)H20] • 2 H20 (2 a), which contain the first reported isopoly-thioanion of a transition metal have been determined: la: (PI, a = 913.0(1), b = 1000.1(2), c = 1333.9(2) pm, a = 87.11(1), ß = 85.18(1), v = 83.07(1)°, V = 1277.0 • 10 6 pm 3 , Z = 1); ' 2a: (P2i/n, a = 071.0(2), b = 2018.5(4), c = 714.4(2) pm, ß = 101.42(2)°, V -949,3 • 10 6 pm 3 , Z = 2) and compared with that of the trimetallic heteropoly-thioanion of (AsPh4)2[(WS4)Ni(WS4)] (3a). 3a: (PI. a = 1255.2(3), b = 1277.1(3), c = 939.0(2) pm, a = 113.19(2), ß = 90.28(2), y = 108.72(2)°, V= 1201.5-10 6 pm 3 , Z = 1). Though there are delocalized orbitals in the isopoly-thioanions they can be regarded as coordination compounds of W IV X 2+ containing two W VI S4 2 ~ ligands. 
  Reference    Z. Naturforsch. 37b, 1014 (1982); eingegangen am 6. April 1982 
  Published    1982 
  Keywords    Crystal Structure, Isopoly-Thioanions, Heteropoly-Thioanions, Thiometalates, Mixed Valence Compounds 
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 Identifier    ZNB-1982-37b-1014 
 Volume    37 
30Author    Antonios Antoniadis, Wolfgang Hiller, Udo Kunze, Schaal Herberth, Joachim SträhleRequires cookie*
 Title    Phosphinsubstituierte Chelatliganden, VI [1] Kristallstrukturen von Tetracarbonyl(diphenylphosphino -N-phenylthioformimidato -P,S )mangan(I) und Tetracarbonyl(diphenylthiophosphoryl-N-phenylthioformimidato-S,S')mangan(I) Phosphine Substituted Chelate Ligands, VI [1] Crystal Structures of Tetracarbonyl(diphenylphosphino-N-phenylthioformimidato-P,S)- manganese(I) and Tetracarbonyl(diphenylthiophosphoryl-X-phenylthioformimidato-S.S')- manganese(I)  
 Abstract    The phosphinothioformimidato complex (CO)4MnSC(NPh)PPli2 (1) crystallizes tri-clinic in the space group PI with lattice constants a = 989.4(9) pm, b — 1042.0(8) pm, c = 1088.5(8) pm, a = 91.45(4)°, ß = 97.10(4)°, y = 100.53(5)°. The four-membered chelate I 1 ring Mn-P-C-S is folded over the P-S edge by a dihedral angle of 167.1°. The crystal I 1 system of the thiophosphoryl thioformimidato complex (CO)4MnSC(NPh)P(S)Ph2 (2) is monoclinic with the space group P2i/c, and the lattice parameters are a = 1109.5(3) pm, b = 966.0(3) pm, c = 2256.7(3) pm, 0=103.11(2)°. The chelate ligand is linked to the metal by two S atoms forming a five-membered ring in the "envelope" conformation with the thiophosphoryl S atom at the apical position. 
  Reference    Z. Naturforsch. 37b, 1289—1293 (1982); eingegangen am 7. Mai 1982 
  Published    1982 
  Keywords    Crystal Structure, Chelate Ligands, Phosphinothioformimidate, Thiophosphorylthioformimidate, Manganese Complexes I 1 
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 Identifier    ZNB-1982-37b-1289 
 Volume    37 
31Author    H.-J Schweizer, Reginald GruehnRequires cookie*
 Title    Zur Darstellung und Kristallstruktur von ß-Nb02 Synthesis and Crystal Structure of /?-Nb02  
 Abstract    By using chemical transport reactions with various transporting agents (HgCl2, NbCls, Nb3C>7Cl) a slightly substoichiometric NbCVphase, ß-NbOz, was obtained from samples with O/Nb ~ 1.5 (source; T > 1373 K) and with deposition temperatures > 1273 K (sink). The range of composition of ß-NbC>2 was found to exist from NbOi.990 to NbOi.998. The structure of the tetragonal, column-shaped black crystals was determined by X-ray diffraction. It crystallizes tetragonally in the space group I4i with lattice constants a = 9.693(3) A, c = 5.985(1) A and Z = 16 formula units. The crystal structure of /?-NbC>2 is shown to be a deformed rutile type. As in a-NbÜ2 the Nb-atoms are grouped in pairs. However, both oxides are different with respect to their long-range order. 1. Einleitung Neben a-Nb02 [1, 2, 3], dessen Struktur seit 20 Jahren bekannt ist [4-6] und das eine Phasen-umwandlung in a'-Nb02 [7] zeigt, wurde von R. Gruehn [8-10] beim Erhitzen von Nb/Nb205-Gemengen mit O/Nb < 2,0 unter Zusatz eines Mineralisators (NbaOyCl) eine weitere Dioxidphase /?-Nb02 reproduzierbar erhalten. Das Guinier-Dia-gramm der neuen Phase ließ sich mit Hilfe der Methode von P. M. De Wolff [11] tetragonal indi-zieren [8]. Heterogene Gemenge aus a-und ß-Nb02 (max. 1:1) konnte D. Bergner [12] durch Reduktion von Nb20s-Pulver mit definierten H2/H20-Gas-mischungen (Eis/Wasser-Mischung, Elektrolytwas-serstoff, T = 1523 K) darstellen. Das vereinzelte Auftreten von /5-Nb02-Einkristal-len bei Transportexperimenten (NbO/NbO^-Aus-gangsbodenkörper, Transportmittel Iod [13]) er-möglichte W. Mertin [14] eine erste strukturelle Charakterisierung der neuen Dioxidphase. Nach Weißenberg-und Präzessionsaufnahmen kristalli-siert /?-Nb02 wie die a-Form in der Raumgruppe I4i/a; die aus den Einkristallaufnahmen ermittel-ten Gitterkonstanten betragen ao — 9,68 A; Co = 5,975 Ä; vgl. Abschn. 4. Von H. Schäfer et al. [9] wurde darauf hingewie-sen, daß /?-Nb02 stets neben NbO auftritt; die Zu-sammensetzung wurde zu 2,000 ± 0,001 O/Nb be-stimmt und ein reversibler Übergang in /?'-Nb02 
  Reference    Z. Naturforsch. 37b, 1361—1368 (1982); eingegangen am 9. Juli 1982 
  Published    1982 
  Keywords    Substoichiomotric NbC>2, Synthesis by Chemical Transport, Crystal Structure 
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 Identifier    ZNB-1982-37b-1361 
 Volume    37 
32Author    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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 Identifier    ZNB-1982-37b-1437 
 Volume    37 
33Author    Rudolf Allmann, Eberhard Hohaus, Stanislaw 01ejnikRequires cookie*
 Title    Boron Chelates and Boron-Metal Chelates, X [1] 3-(2-Hydroxyphenyl)-2,2-diphenyl-l-oxa-3-azonia-2-borata-naphthalene- methanol (1/1): Synthesis, Spectroscopic Investigations and Crystal Structure  
 Abstract    2-Aminophenol, salicylaldehyde and diphenylboric anhydride react in methanol to form a fluorescent, chelate-like azomethineboron compound containing methanol. The title compound, C25H20BNO2 • CH3OH, was examined by UV, IR, HI, and NMR spectroscopy as well as by thermogravimetry and X-ray structure analysis (Pbnb, a= 8.815, b= 17.309, c = 28.992 Ä, R = 5.5%). These investigations show the six-membered chelate ring (chelate A) to exist as formulated in [2] and not as a five-membered chelate ring B. One methanol molecule connects two chelate molecules by hydrogen bonds, resulting in an overall ratio of chelate to methanol of 1 : 1. 
  Reference    Z. Naturforsch. 37b, 1450—1455 (1982); received May 1 O/June 11 1982 
  Published    1982 
  Keywords    Boron Chelate, Azomethine, Crystal Structure, UV Spectra, NMR Spectra 
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 Identifier    ZNB-1982-37b-1450 
 Volume    37 
34Author    HerbertW. Roesky, Habibollah Djarrah, Mathias Noltemeyer, GeorgeM. SheldrickRequires cookie*
 Title    Über Reaktionen von Pyrrolidinium-bis(diethylphosphoryl)phosphinidin mit Chromcarbonylkomplexen Reaction of Pyrrohdinium-bis(diethylphosphoryl)phosphinidine with Chromiumcarbonyl Complexes  
 Abstract    The reaction of [H2NC4H8]P[P(0)(0C2H5)2]2 with Cr(CO)5THF and Cr(CO)4C7H8 results in the formation of the 1: 1 and 1:2 chromium pentacarbonyl complexes. The 1: 1 complex was characterized on the basis of an X-ray analysis. It crvstallizes in the space group P I with a = 1091.9(10), 6=1164.1(12), c ='l356.4(9) pm, a = 108.89(6), ß= 97.57(7), y = 116.24(6), and Z — 2. The average P-P bond length was found to be 215.8 pm. 
  Reference    Z. Naturforsch. 37b, 1580—1583 (1982); eingegangen am 9. August 1982 
  Published    1982 
  Keywords    Crystal Structure, 31 P NMR Spectra, Phosphorus-Phosphorus Bonds, Chromium 
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 Identifier    ZNB-1982-37b-1580 
 Volume    37 
35Author    Gerhard Cordier, Gerhard Savelsberg, Herbert SchäferRequires cookie*
 Title    Zintlphasen mit komplexen Anionen: Zur Kenntnis von Ca3AlAs3 und Ba3AlSb3 Zintl Phases with Complex Anions: On Ca3AlAs3 and Ba3AlSb3  
  Reference    Z. Naturforsch. 37b, 975—980 (1982); eingegangen am 10. März 1982 
  Published    1982 
  Keywords    Calcium-Arsenoaluminate, Barium-Antimonoaluminate, Crystal Structure, Intermetallic Phases of the Zintl-type 
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 Identifier    ZNB-1982-37b-0975 
 Volume    37 
36Author    Marianne Baudler, Yusuf Aktalay, Thomas Heinlein, Karl-Friedrich TebbeRequires cookie*
 Title    Contributions to the Chemistry of Phosphorus, 109 [1] J-BueAs2P6 -the First Phosphorus Arsenic Polycycle  
  Reference    Z. Naturforsch. 37b, 299—305 (1982); eingegangen am 12. Oktober 1981 
  Published    1982 
  Keywords    2, 2', 3, 3', 4, 4'-Hexa-ter<-butyl-l, l / -diarsa-2, 2', 3, 3', 4, 4'-hexaphospha-bicyclobutane, Phosphorus Arsenic Polycycle, Heterocyclophosphanes, Crystal Structure 
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 Identifier    ZNB-1982-37b-0299 
 Volume    37 
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