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1985 (35)
21Author    Claudia FriedrichRequires cookie*
 Title    Zur Stereochemie des freien Elektronenpaares in Verbindungen des vierwertigen Tellurs: Verzerrtes TeCI62"-Oktaeder in |H  
 Abstract    ,N (C H 2),NH3lTeCI," regulär oktaedrisches Anion in | HjINfCHjliNHilSnCI,, On the Stereochemistry of Lone Pair Electrons in Com pounds with Tetravalent Tellurium: D istorted TeCl62~-Octahedron in [H3N (C H 2)3N H 3]T eCl6, Regular Octahedral A nion in [H3N (C H 2)3N H 3]SnC l6 W alter Abriel* Using 293 K diffractom eter intensity data, the structures o f [H 3N (C H 2)3N H 3]TeCl6 and [H3N (C H 2)3N H 3]SnCl6 have been determ ined by single crystal X-ray technique and refined to a 
  Reference    Z. Naturforsch. 40b, 1691 (1985); eingegangen am 30. August 1985 
  Published    1985 
  Keywords    Lone Pair Electrons, Tellurates, Stannates, Crystal Structure 
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 Identifier    ZNB-1985-40b-1691 
 Volume    40 
22Author    Joachim Pickardt, Pamela DroasRequires cookie*
 Title    Metal Complexes with Hexamethylenetetramine as a Ligand, V II [1] Crystal Structures of the Zinc Chloride Adduct ZnC l2 * C6H 12N4, and the Zinc Bromide Adduct ZnBr2 * C6H 12N4  
 Abstract    By reaction of zinc chloride and zinc bromide with hexamethylenetetramine in water/methanol crystals of the adducts Z nC l2 • C6H 12N 4 and ZnBr2 • C6H I2N4, resp. were obtained. The compounds are isotypic, they crystallize in the orthorhombic space group P2,am (non-standard setting of space group Pmc2,, No. 26), Z = 2. The lattice parameters of the zinc chloride adduct are a = 1168.0(4), b = 685.7(4), and c = 601.1(4) pm, of the zinc bromide adduct a — 1188.9(6), b = 721.5(5), and c = 602.3(4) pm. The adducts are polymeric, they form parallel chains in the crystal. The zinc atoms are bonded to two halo­ gen atoms and, via nitrogen atoms, to two hexa­ methylenetetramine molecules, which act as biden-tate ligands. The coordination of the zinc atoms is approximately tetrahedral. 
  Reference    Z. Naturforsch. 40b, 1756—1758 (1985); eingegangen am 18. Juli 1985 
  Published    1985 
  Keywords    Hexamethylenetetramine, Zinc Chloride Adduct, Zinc Bromide Adduct, Crystal Structures 
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 Identifier    ZNB-1985-40b-1756_n 
 Volume    40 
23Author    Horst Sabrowsky, Alfred Thimm, Petra Vogt-M, ErtensRequires cookie*
 Title    NaLiS: Ein weiteres Interalkalimetallsulfid NaLiS: A nother Inter Alkaline M etal Sulphide  
 Abstract    The colourless com pound NaLiS has been prepared and its structure determ ined by single crystal X-ray diffraction techniques. The very hygroscopic NaLiS crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a = 402.6(1), c = 649.5(2) pm. The structure was solved from 720 counter reflections (216 symmetry independent re­ flections) by differential Fourier syntheses. Refining gives a least squares residue of 0.024. The a«/z'-PbFCl-type structure is characterized by layers o f LiS4/4-tetrahedra connected by their edges in two dim ensions and 2 interspersed layers of sodium. 
  Reference    Z. Naturforsch. 40b, 1759 (1985); eingegangen am 19. A ugust 1985 
  Published    1985 
  Keywords    Sodium Lithium Sulphide, Crystal Structure, X -R ay 
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 Identifier    ZNB-1985-40b-1759_n 
 Volume    40 
24Author    Udo Kunze, Hussain Jawad, Wolfgang Hiller, Regina NaumerRequires cookie*
 Title    Phosphinsubstituierte Chelatliganden, XIV [1] Wasserstoff-Brückenbindung in THF-Addukten von Tetracarbonylchrom-und -molybdänkomplexen mit P,S-koordinierten Phosphinothioformamid-Liganden. Kristallstruktur von [(CO) 4 Cr(PPh 2 C(S)NHMe)] THF Phosphine-Substituted Chelate Ligands, XIV [1] Hydrogen Bonding in THF-Adducts of Tetracarbonylchromium and -molybdenum Complexes with P,S-Coordinated Phosphinothioformamide Ligands. Crystal Structure of [(CO) 4 Cr(PPh 2 C(S)NHMe)] * THF  
 Abstract    The tetracarbonyl chromium and molybdenum P,S-chelate complexes la, b and 2a, b are obtained by low-temperature photolysis of the metal hexacarbonyls with the neutral phos-phinothioformamide ligands, Ph 2 PC(S)NHR (R = Me (a), Ph (b)), as stoichiometric 1/1 THF adducts. A weak N-H---O(THF) hydrogen bond is deduced from the ; H NMR spectra which show a collapse of the N-methyl doublet in la (T c -18 °C) but not in 2a. Unusually small P-C(S) couplings are observed in the 13 C{'H} NMR spectra. The N-methyl chromium complex la crystal-lizes in the triclinic space group P1 (Z = 2) with the lattice constants a = 1076.6(3), b = 1235.8(3), c = 915.1(3) pm, a = 97.99(4)°, ß = 92.73(5)°, y = 87.63(5)°. The planar thioamide unit adopts the Z configuration and is linked to the tetrahydrofuran molecule by a hydrogen bond (N-H1-031 164°) with an 0---H contact distance of 191 pm. 
  Reference    Z. Naturforsch. 40b, 512—517 (1985); eingegangen am 23. November 1984 
  Published    1985 
  Keywords    Hydrogen Bonding, THF-Adducts, Phosphinothioformamide Complexes, Crystal Structure, Chromium Complex 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0512.pdf 
 Identifier    ZNB-1985-40b-0512 
 Volume    40 
25Author    Schäfer, Michael SteherRequires cookie*
 Title    Neue Zintlphasen: Ba3GaSb3, Ca3GaAs3 und Ca3InP3  
 Abstract    The new compounds Ca3G aA s3 and Ca3InP3 crystallize in the orthorhom bic system, space group Pnm a (No. 62) with the lattice constants 
  Reference    Z. Naturforsch. 40b, 1100—1104 (1985); eingegangen am 3. Juni 1985 
  Published    1985 
  Keywords    C alcium -Inoarsenidogallate, Calcium -Inophosphidoindate, B arium -Soroantim onidogallate, Crystal Structure 
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 Identifier    ZNB-1985-40b-1100 
 Volume    40 
26Author    Wolfgang Saak, Siegfried PohlRequires cookie*
 Title    lodsubstituierte Eisen-Schwefel-Cluster: Neue Synthesen sowie zur Bildung und Stabilität von Fe2S2I42-, Fe4S4I42_ und Fe6S6I62-. Die Kristallstruktur von (Et4N)6(Fe4S4l4)2Fe2S2l 4 Iodine Substituted Iron-Sulfur-Clusters: Novel Syntheses, Form ation and Stability of Fe2S2I42_, Fe4S4l 42_, and Fe6S6I62~. The Crystal Structure of (E t4N)6(Fe4S4l4)2Fe2S2l4  
 Abstract    Fe4S4I42~ has been prepared in tetrahydrofuran (TH F) solution by the reaction of Fe, S8, I2, and Me3N CH 2PhTI~, and isolated as black, fairly air-stable crystals of (M e3N CH 2P h)2Fe4S4I4 (1) in nearly quantitative yield. 1 reacts with iron and iodine or with elem ental sulfur and F e l2 in C H 2C12 solution to form Fe6S6I62~ which was isolated as black crystals of (M e3N C H 2P h)2Fe6S6I6 (5). In T H F solution Fe6S6I62-is converted to Fe4S4I42~ which was isolated as Fe(T H F)6Fe4S4I4-4 TH F (3). Evidence is presented for an equilibrium betw een Fe2S2I42~ and Fe4S4I42_, F el42~ and sulfur when iron, sulfur, iodine and E t4N +I~ react (with the required stoichiom etry) to form Fe2S2I42_ in C H 2C12 solution. From this solution (E t4N)6(Fe4S4I4)2Fe2S2I4 (6) crystallizes as black needles 
  Reference    Z. Naturforsch. 40b, 1105 (1985); eingegangen am 9. A pril/29. Mai 1985 
  Published    1985 
  Keywords    Iodine Substituted Iron-Sulfur Clusters, Novel Syntheses, Stability, Crystal Structure 
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 Identifier    ZNB-1985-40b-1105 
 Volume    40 
27Author    Rolf Minkwitz, UlrikeN. Aß, Armin Radünz, Hans PreutRequires cookie*
 Title    Beiträge zur Chemie der Schwefelhalogenide, 9 [1]  
 Abstract    Trifhiormethyldichlorsulfonium(IV)-hexafluoroarsenat(V) Contributions to the Chemistry of Sulfur Halides, 9 [1] Trifluorom ethyldichlorosulfonium (IV) H exafluoroarsenate(V) The synthesis of CF3SC12+A sF6_ is reported. The sulfonium salt is characterised by IR , Ram an, l9F and l3C NMR spectroscopy. The vibrational assignment is based on a Cs model for the cation and assisted by a normal coordinate analysis. The crystal structure has been determ ined from three-dimensional diffractom eter data at —133 K. The structural data for the cation are: C -F = 128.8(5) pm, C -S = 197,8(3) pm, S -C l -195,9(1) pm and F -C -F -111,8(3)°, C l -S -C l = 104,22(5)°, C -S -C l -99,8(1)°. 
  Reference    Z. Naturforsch. 40b, 1123—1129 (1985); eingegangen am 6. Mai 1985 
  Published    1985 
  Keywords    Preparation, Crystal Structure, Bonding and Force C onstants, Sulfur Halides 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1123.pdf 
 Identifier    ZNB-1985-40b-1123 
 Volume    40 
28Author    Martin Schabert, Gerhardt PausewangRequires cookie*
 Title    Darstellung, Kristallstruktur und spektroskopische Daten von Rb2VOF4 Preparation, Crystal Structure and Spectroscopic Data o f R b2V O F 4  
 Abstract    Crystals o f R b 2V O F 4 have been obtained under hydrothermal conditions. The crystal structure (orthorhom bic, space group Pnma, a = 759.9(2) pm, b = 579.1(2) pm, c = 1193.8(4) pm, Z = 4, dc = 3.96 gem -3, dm = 3.90 gem-3, R — 0.019 for 655 independent reflections) shows infinite zig-zag-chains o f V O F 5-octahedra along the 6 -axis, linked by c/j-bridging F-atoms. Despite o f orien­ tational disorder, clear evidence for a trans-effect could be established: d (V —O) 165.8(2), d (V —F,rans bridge) 221.1(1), d (V -F cu bridge) 203.6(1), d (V -F term inal) 185.2(2), 187.8(2), 193.2(2) pm. 
  Reference    Z. Naturforsch. 40b, 1437—1440 (1985); eingegangen am 9. Juli 1985 
  Published    1985 
  Keywords    R b 2V O F 4, Crystal Structure, Preparation, Spectroscopic Data 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1437.pdf 
 Identifier    ZNB-1985-40b-1437 
 Volume    40 
29Author    HeribertW. Adle, Elke Conradi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Cyclothiazeno-oxo-diazidowoIframat(VI) Die Kristallstruktur von (AsPh4)2[W(N3S2)(0)(N3)2]2 Cyclothiazeno Oxodiazidotungstate(VI) The Crystal Structure of (A sPh4)2[W (N3S2)(0 )(N 3 )2]2  
 Abstract    A new, im proved m ethod of synthesis for the cyclothiazeno complex A sPh4[WCl4(N 3S2)] con­ sists of the reaction of Na2W 0 4 with molten trithiazyl chloride (NSC1)3 followed by treatm ent with A sPh4Cl in C H 2C12. Through the reaction with silver azide suspended in C H 2C12 in the presence of m oisture, black crystalline (A sPh4)2[W(N3S2)(0)(N 3)2]2 is obtained. Its IR spectrum and its crys­ 
  Reference    Z. Naturforsch. 40b, 1626—1630 (1985); eingegangen am 28. A ugust 1985 
  Published    1985 
  Keywords    Cyclothiazeno O xodiazidotungstate(V I), Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1985-40b-1626 
 Volume    40 
30Author    Hans-U HummelRequires cookie*
 Title    Zur Darstellung und Kristallstruktur von Barium-l,l-dicyanoethylen-2,2-oxo-thiolat-Tetrahydrat — ein Salz mit dem Anion [0(S)CC(CN) 2 ] 2 " Synthesis and Crystal Structure of Barium-l,l-dicyanoethylene-2,2-oxo-thiolate Tetrahydrate — a Salt with the Anion [0(S)CC(CN) 2 ] 2 ~  
 Abstract    By reaction of COS with malonitrile in presence of potassium ethanolate in ethanol K 2 0(S)CC(CN) 2 • H : 0 is obtained. It reacts with Ba(NCS) 2 -3H 2 0 in ethanol to form colourless crystals of BaO(S)CC(CN) 2 • 4H : 0. The space group of the barium salt is Pn2,a (standard: Pna2,) with Z = 4. The structure consists of Ba 2+ and [0(S)CC(CN) 2 ] 2 ~ ions. The barium ion is bound to three nitrogen and six oxygen atoms. The coordination polyhedron is a tricapped trigonal prism. The anion [0(S)CC(CN) 2 ] 2 ~ is not exactly planar and is involved in several hydrogen bondings. 
  Reference    Z. Naturforsch. 40b, 722—725 (1985); eingegangen am 11. Februar 1985 
  Published    1985 
  Keywords    Barium-1, l-dicyanoethylene-2, 2-oxo-thiolate Tetrahydrate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1985-40b-0722 
 Volume    40 
31Author    U. W. Becker, J. Felsche, G. Huttner, O. ScheidstegerRequires cookie*
 Title    Preparation and Crystal Structure of a New Mixed Valence Cerium Germanate Ce2 + Ce! + [Ge0 4 ]3[Ge20 7 ]2[Ge 3 0 1 o]  
 Abstract    Opaque blue crystals of a new mixed valence cerium germanate have been prepared at elevated temperatures (1555 K) under careful thermoanalytical control. Single crystal structure analysis shows three different types of germanate anions [Ge0 4 ] 4 ~, [Ge 2 0 7 ] 6 ~ and [Ge 3 O 10 ] 8 ~, all ger-manium atoms being in tetrahedral coordination. Due to the larger number of oxygens per unit cell (Ce 2 Ge 2 0 72), with all the oxygens unambiguously located by X-ray single crystal structure analysis, this phase differs significantly from the corresponding cerium(III) germanate Ce 2 Ge 2 0 7 , which shows [Ge0 4 ] 4_ and [Ge 3 Oi 0 ] 8 ~, but no [Ge 2 0 7 ] 6 ~ ditetrahedral groupings. 
  Reference    Z. Naturforsch. 40b, 755—761 (1985); received January 30/March 3 1985 
  Published    1985 
  Keywords    X-Ray, Crystal Structure, Mixed Valence Cerium, Heavy Atom Layer Structure, Thermoanalysis 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0755.pdf 
 Identifier    ZNB-1985-40b-0755 
 Volume    40 
32Author    KlausD. Ieter Scherfise, FrankW. Eller, Kurt DehnickeRequires cookie*
 Title    Die  
 Abstract    Kristallstrukturen von [(CH3)P(C6H5)3][C(N02)3] und [(ICH2)P(C6H5)3][C (N 0 2)3] Crystal Structures of [(CH3)P(C6H ?)3][C(N0 2)3] and [(IC H 2)P(C 6H 5)3][C(N 0 2)3] The title compounds and the trinitro methanide salts with PPh4~ and N-methyl pyridinium cations are prepared from K[C(NOi)3] and the chlorides of the organic cations in aqueous solu­ tion. They form thermally stable, yellow crystalline solids. The IR spectra are reported. The crystal structures of [(CH3)P(C6H 5)3][C(N0 2)3] (2) and [(ICH2)P(C6H 5)3][C(N0 2)3] (3) are deter­ mined by the aid of X-ray methods. 2: space group P2,/c, Z = 4; a = 825, b = 1404, c = 1771 pm; ß = 97.4°; 1891 independent observed reflexions. R — 0.063. 3: space group P 2t/c, Z = 4; a = 848, b = 1364, c -1869 pm; ß = 99.9°; 2380 independent observed reflexions. R = 0.036. Both compounds are ionic and consist of [(CH3)P(C6H5)3]® and [(ICH2)P(C6H5)3] cations, resp., without special features, and trinitro methanide ions. In the anions the carbon atoms are almost coplanar with the N-atoms of the nitro groups with mean C -N bond lengths of 139 pm and mean NCN bond angles of 120°, suggesting sp2 hybridisation. In 3 the torsional angles between CN3 plane and the N 0 2 groups range from 15° to 32°, whereas in 2 two of the N 0 2 groups are almost coplanar with the CN3 moiety (dihedral angles 0.3° and 8.1°) and one nitro group is disordered in two positions (dihedral angles 15.8° and 74.7°). 
  Reference    Z. Naturforsch. 40b, 906—912 (1985); eingegangen am 10. April 1985 
  Published    1985 
  Keywords    (Methyl)triphenylphosphonium Trinitromethanide, (Iodomethyl)triphenylphosphonium Trinitromethanide, Preparation, Crystal Structure, IR Spectra 
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 Identifier    ZNB-1985-40b-0906 
 Volume    40 
33Author    Jürgen Hanich, Wolfgang Willing, Ulrich Müller, Kurt Dehnicke, Dieter RehderRequires cookie*
 Title    Cyclothiazeno-Vanadiumdibromid, VBr2(N3S2) Cyclo-Thiazeno Vanadium Dibromide, V B r2(N 3 S2)  
 Abstract    V B r 2(N 3S2) was synthesized by reaction o f VC12(N 3S2) with M e 3SiBr. It reacts with PPh4B r in dibromomethane solution to form (P P h 4) 2[V B r 3(N 3S2) ] 2. The compounds were characterized by their IR and 51V N M R spectra. The crystal structure o f V B r 2(N 3S2) was determined by X-ray diffraction (2060 reflexions, R = 0.114). Crystal data: triclinic, space group P I , a — 586.4, b = 794.2, c — 744.6 pm, a = 89.25, ß = 108.58, y — 99.67°, Z = 2. The vanadium atoms form planar, six-membered rings with the N 3S2 groups, with short V N distances (172 and 185 pm). Bromine-bridged dimers are associated via V —N links to form chains in a similar way as in some tetrahalides. The structure is similar to that o f VC12(N 3S2), but the chains are rotated by 17° along their axes. 
  Reference    Z. Naturforsch. 40b, 1457—1462 (1985); eingegangen am 2. Juli 1985 
  Published    1985 
  Keywords    Cyclo-Thiazeno Vanadium Dibrom ide, Synthesis, IR Spectra, 51V N M R Spectra, Crystal Structure 
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 Identifier    ZNB-1985-40b-1457 
 Volume    40 
34Author    Achim Müller, Erich Krickemeyer, Rainer Jostes, Hartmut Bögge, Ekkehard Diemann, Ulrich BergmannRequires cookie*
 Title    Über [Co4S3 (SO)(CN)12]8 : bemerkenswerte Bildung eines Clusters und eines "SO"-Liganden sowie Relevanz zum Promotor-Effekt bei der HDS-Katalyse [Co4S3(SO )(CN )12]8-: A Remarkable Formation of a Cluster and a "SO " Ligand and its Relevance to the Promotor Effect of HDS Catalysis  
 Abstract    The preparation of K8[Co4S3(SO)(C N)12] • 4 H 20 (by cyanolysis of "cobalt sulfide") and its properties (vibrational, U V/VIS and ESCA spectra, magnetic and thermogravimetric data, and crystal structure) are reported. The formation of a "SO " ligand through air oxidation is discussed with regard to the promoting effect of Co in the CoMoS phase of the hydrodesulfurization (HDS) catalyst. 
  Reference    Z. Naturforsch. 40b, 1715 (1985); eingegangen am 24. Juni/18. September 1985 
  Published    1985 
  Keywords    Sulfido Cluster, Metal Sulfides, HDS (Hydrodesulfurization) Catalysis, Crystal Structure, Amorphous Substances 
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 Identifier    ZNB-1985-40b-1715 
 Volume    40 
35Author    Winfried Hinrichs, Jürgen Kopf, Klaus-Wilhelm Stender, Günter KlarRequires cookie*
 Title    Selbststapelnde Systeme, I 4 a Compound with Radical Cations and Polyiodide Chains  
 Abstract    ,4' ,5,5'-Tetramethoxy-2,2'-dithiobiphenyl-Iod (6/7), eine Verbindung mit Radikalkationen und Polyiodidketten Selfstacking Systems, I 4,4',5,5'-Tetramethoxy-2,2'-dithiobiphenyl-Iodine (6/7), 
  Reference    (Z. Naturforsch. 40b, 39—44 [1985]; eingegangen am 20. September 1984) 
  Published    1985 
  Keywords    4, 4', 5, 5'-Tetramethoxy-2, 2'-dithiobiphenyl-Iodine (6/7), Molecular and Crystal Structure, Self-stacking Systems, Polyiodide Chains 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0039.pdf 
 Identifier    ZNB-1985-40b-0039 
 Volume    40 
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