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Facet   section ZfN Section B:Volume 042  [X]
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1987 (30)
21Author    Brigitte Eisenmann, Roland ZaglerRequires cookie*
 Title    [Ba(en)4]2As4Te6, das erste Telluridoarsenat(II) [B a(en)4 ]2 As4Te6, the First Telluridoarsenate(II)  
 Abstract    The new com pound [B a(en)4]2A s4T e6 has been prepared by reaction of appropriate mixtures of the elem en ts in dry ethylenediam ine. It crystallizes in the m onoclinic system , space group P 2,/« with a = 1776.0(6) pm, b = 1459.9(6) pm, c = 1000.0(4) pm, ß = 101.8(1)°. The A s4T e64~ anion forms a six-m em bered ring A s4T e2 o f chair conform ation, in which two A s —A s groups are bridged by Te atom s. A t each A s atom a further exocyclic Te neighbour is bonded in the equatorial position. The Ba2+ cation is eight-coordinated by the bidentate ethylenediam ine ligand. 
  Reference    Z. Naturforsch. 42b, 1079—1082 (1987); eingegangen am 1. Juni 1987 
  Published    1987 
  Keywords    Telluridoarsenate, Semimetal A nion, Crystal Structure Preparation 
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 Identifier    ZNB-1987-42b-1079 
 Volume    42 
22Author    Kay Jansen, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von (PPh4)2[Mo2(02C—Ph)4Cl4] * 2 CH2C12, einem Komplex mit Mo=Mo-Bindung Synthesis and Crystal Structure of (PPh4 )2 [Mo2 (0 2 C —Ph)4 Cl4] -2 CH 2 C12, a Complex with M o=M o Bonding  
 Abstract    The title com pound has been prepared from (PPh4)2[M o2(0 2C —Ph)4Cl2] and CC14 in C H 2C12 solution as moisture sensitive crystals, which are black in reflexion and yellow in transmission. (PPh4)2[M o2(0 2C —Ph)4Cl4] • 2 C H 2C12 was characterized by a X-ray crystal structure determ ination (7873 observed independent reflexions, R = 0.048). It crystallizes in the space group P 1 with one formula unit in the unit cell; the lattice constants are a = 1186.4; b = 1404.0; c = 1451.0 pm; a = 61.98°; ß = 78.91°; y = 78.26°. The structure consists o f PPh4® ions, C H 2C12 m olecules and centrosym m etric anions [M o2(0 2C —Ph)4Cl4]20 containing a molybdenum d3d3 unit with a relatively long M o = M o bond o f 249.6 pm. The M o= M o group is spanned in a chelate manner by four O atoms of two benzoate groups and by two further single O atoms o f two further benzoate groups. Two terminal Cl atom s on each Mo atom com plete the pentagonal bipyramidal coordination spheres about the Mo atoms. 
  Reference    Z. Naturforsch. 42b, 1097—1101 (1987); eingegangen am 2. März 1987 
  Published    1987 
  Keywords    Tetrabenzoato-tetrachloro-dim olybdate, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1097.pdf 
 Identifier    ZNB-1987-42b-1097 
 Volume    42 
23Author    D. Ietm Ar Stalke, Nayla Keweloh, Uwe Klingebiel, M. Atthias, N. Oltem Eyer, G. Eorge, M. SheldrickRequires cookie*
 Title    Von lithiierten Aminofluorsilanen zu mono-und dimeren Iminosilanen From Lithiated Aminofluorosilanes to Mono-and Dimeric Iminosilanes  
 Abstract    Depending on the solvent and the bulkiness of the substituents, lithiated aminofluorosilanes are dimers, monomers, or LiF-adducts of iminosilanes. In the crystal structure of the dimeric lithium derivative of di-terr-butyl(/m-butylamino)fluorosilane, each lithium atom is coordinated by one fluorine and two nitrogen atoms. LiF-elimination leads — if sterically possible — to dimerisation. The limits of dimerisation are reached with the dimer diisopropyl(trwm-butylphenyl-imino)silane, for which the crystal structure analysis shows severe steric distortions. Fluorine-chlorine-exchange occurs in reactions of lithiated (tri-fm-butylphenylimino)fluorosilanes with Me3SiCl. Iminosilanes are obtained by thermal LiCl-elimination from the resulting salts. 
  Reference    Z. Naturforsch. 42b, 1237—1244 (1987); eingegangen am 4. Mai/25. Juni 1987 
  Published    1987 
  Keywords    Aminofluorosilanes, Lithium Salts, Cyclisation, Iminosilanes, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1237.pdf 
 Identifier    ZNB-1987-42b-1237 
 Volume    42 
24Author    Peter Schreiber, Karl Wieghardt, Ulrich Flörke, Hans-Jürgen HauptRequires cookie*
 Title    Synthese von Wolframkomplexen  
 Abstract    des Typs [ L W (C O) 3X ] + (X = H , F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [L W (C O) 3B r]B F 4 und [L W (C O) 3H ] 2[W O C l5] • h 2o Synthesis o f Tungsten Complexes o f the Type [L W (C O)3X ] + (X = H, F, Br; L = 1.4,7-triazacyclononane). The Crystal Structures o f [L W (C O)3Br]BF4 and [L W (C O)3H ]2[W O C l5] • H 20 The reaction of LW (C O), (L = 1,4,7-triazacyclononane) with Br2 in CHCl, yields orange [L W (C O)3Br](Br3) which was converted to its BF4~ salt. [L W (C O)3Br]BF4 crystallizes in the triclinic space group P 1 (a = 8.273(3), b = 8.628(2), c = 13.034(3) Ä , a = 80.10(2), ß = 72.69(2). y = 61.14(2)°, Z = 2); it consists of cations [L W (C O)3Br] + , with seven-coordinate W atoms, and BF4 -anions. The corresponding salt [L W (C O)3F](PFft) was obtained from L W (C O)3 with 20% aqueous HF in the presence of air and addition of NaPF6. The analogous reaction with 37% aqueous HC1 affords green crystals of [L W (C O)3H ]2[W OCl5] • H 20 which crystallize in the mono­ clinic space group P2,/c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Ä . ß = 105.65(3)°, Z — 4). The W atoms in the [L W (C O)3H ]+ cations are seven-coordinate; the six-coordinate [W OCl5]: anions are not disordered. The W = 0 distance is short (1.72(1) Ä), the mean equatorial W —Cl distance is 2.390 Ä whereas the W —Cl bond distance trans to the W = 0 group is 2.562(5) Ä. 
  Reference    Z. Naturforsch. 42b, 1391 (1987); eingegangen am 2. Juli 1987 
  Published    1987 
  Keywords    Tungsten Complexes, X-Ray, Crystal Structure 
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 Identifier    ZNB-1987-42b-1391 
 Volume    42 
25Author    D. Ieter, F. Enske, PaulM. Aue, K. Urt, M. Erzw EilerRequires cookie*
 Title    Zur  
 Abstract    Reaktion von (f/5-C5H 5)F e(C O)2Br mit Se(SiM e3)2 D ie Kristallstruktur von [S e{F e(C O)2(C5H 5)} 3]2[Fe4Se4Br4] R eaction of (^ -C s H ^ F e ^ O ^ B r with Se(SiM e3) 2 T he C rystal S tructure of [Se {F e (C O)2 (C 5 H 5) } 3 ]2 [Fe4Se4 B r4] 
  Reference    Z. Naturforsch. 42b, 928 (1987); eingegangen am 17. Februar 1987 
  Published    1987 
  Keywords    Synthesis, X -Ray, Crystal Structure of [Fe4Se4B r4]2~-Cluster 
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 Identifier    ZNB-1987-42b-0928_n 
 Volume    42 
26Author    Georg Schmitt, H. Pritzkow, H. P. LatschaRequires cookie*
 Title    Bisdisubstituierte aromatische Phosphane als Komplexliganden Bisdisubstituted A rom atic Phosphanes as Ligands for Metal Complexes  
 Abstract    The photochem ical reaction o f o-CfTT^PF^^; R = O C H 3, O C:H s. m-CftH 4(P R 2)2; R = N (C H 3)2 and /7-C6H 4(P R 2)2; R = O C H ,, N (C H 3)2 with (tricarbonyl)(m ethylcyclopentadienyl)-m anganese (C p ')M n (C O)3 (6) and p-C"H4(P (N (C H 3)2)2)2 with (tricarbonyl)(m ethyl)(cyclopenta-dienyl)m olybdenum (C H 3)(C p)M o(C O)3 (7) yields new manganese and m olybdenum com plexes. o-P henylen-bis(phosphonousaciddim ethylester)(carbonyl)(m ethylcyclopentadienyl)m anganese (8) forms yellow crystals, whose structure is reported. The reaction of o-C 6H 4(P (O C H 3)2)2 (1) with N iC l2 gives a 1:1 phosphane com plex (14), N i(O H)C lopm . The com plexes are characterized by elem ental analysis, 'H N M R , 31P NM R . IR and mass spectroscopy. 
  Reference    Z. Naturforsch. 42b, 1115—1120 (1987); eingegangen am 11. M ärz/14. Mai 1987 
  Published    1987 
  Keywords    C om plexes, P hosphanes, Photochem ical Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1115.pdf 
 Identifier    ZNB-1987-42b-1115 
 Volume    42 
27Author    Ekkehard Fluck3, Gerd Beckerb, Bernhard Neumüllerb, Robert Kneblb, Gem Ot Heckmannb, Heinz RiffelbRequires cookie*
 Title    Ein Derivat des lA5,3A5,5A3-TriphosphabenzoIs A Derivative of lA5,3A5,5A3-Triphosphabenzene  
 Abstract    The title compound was prepared by reacting l,l,3,3-tetrak is(d im eth ylam in o)-lA 5,3A5-diphos-phete with 2,2-dim ethylpropylidynephosphane and characterized by N M R spectra and X-ray structure analysis. 
  Reference    Z. Naturforsch. 42b, 1213—1221 (1987); eingegangen am 19. M ai/16. Juli 1987 
  Published    1987 
  Keywords    lA5, 3A5, 5A3-Triphosphabenzene, NM R Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1213.pdf 
 Identifier    ZNB-1987-42b-1213 
 Volume    42 
28Author    KerstinD. Ippel, NaylaK. Keweloh, P. Eter, G. Jones, Uwe Klingebiel, D.Ieter SchmidtRequires cookie*
 Title    Synthesis and Crystal Structure of a Lithium(trimethylacetoxy-di-terr-butylsilanolate)  
 Abstract    In an acid medium di-tert-butylsilanediol reacts with acyl chlorides to give the di-tert-butyl-chlorosilanol (2) and the carboxylic acid. A lithium salt of a silanol-carboxylic acid ester (5) is formed in the reaction of the lithiated diol with 2,2-dimethylpropionyl chloride. 5 reacts with phenylacetyl chloride to give the first mixed dicarboxyl-silane. The crystal structure determination of 5 shows a Li—O-cubane with C = 0 -Li chelate bonds. 
  Reference    Z. Naturforsch. 42b, 1253—1255 (1987); eingegangen am 16. April/1. Juni 1987 
  Published    1987 
  Keywords    Chlorosilanol, Mixed Silylester, Silanolester, Tetrameric Lithium Salt, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1253.pdf 
 Identifier    ZNB-1987-42b-1253 
 Volume    42 
29Author    Walter AbrielRequires cookie*
 Title    On the Stereochemistry of the Lone-Pair Electrons in AX 6 E-Systems: Dynamically Distorted Anion in (NH 4 ) 2 SeBr 6 , Statically Distorted Anion in l,3-Propanediammonium-Hexabromoselenate(IV) (C 3 N 2 H 12 )SeBr 6  
 Abstract    Using 293 K diffractometer intensity data, the crystal structures of (NH 4) 2 SeBr 6 (1) and [H 3 N(CH 2) 3 NH 3 ]SeBr 6 (2) have been determined by single crystal X-ray technique and refined to a final R w of 0.049 and 0.040, respectively. The dark red crystals of 1 are cubic (space group Fm3m) with a = 10.478(2) Ä and Z = 4. This structure contains SeBe 6 2 ~ octahedra (point symmetry m3m, distance Se —Br: 2.577(2) Ä) in an antifluorite type arrangement of cations and anions. In contrast, the SeBr fi 2-ion in 2 is statically distorted (approximate point symmetry 3m, distance Se-Br min. 2,547(2), max. 2.595(2) Ä. The dark red crystals are orthorhombic (space group Pnma) with a = 17.795(3), b = 7.5037(6), c = 10.476(1) Ä and Z = 4. The results agree with the rules for the appearance of a static/dynamic stereochemical effect of the lone pair electrons given for TeX 6 2 " (X = Cl, Br, I) species (W. Abriel, Acta Crystallogr. B 42, 449 (1986)). Consequently these rules can be extended considering SeX 6 2-as well. Basic structural data for all compounds containing AX 6 2-ions (A = Se, Te; X = Cl, Br, I) known to date are given including the zl-values (R. D. Shannon, Acta Crystallogr. A 32, 751 (1976)) as a measure for the distortion of the octahedral anion. 
  Reference    Z. Naturforsch. 42b, 415—420 (1987); received November 24 1986/January 12 1987 
  Published    1987 
  Keywords    Lone Pair Electrons, Pseudo-Jahn-Teller Effect, Symmetry Rules, Selenates, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0415.pdf 
 Identifier    ZNB-1987-42b-0415 
 Volume    42 
30Author    RolfW. Saalfrank, Franz Schütz, Hans-Ulrich HummelRequires cookie*
 Title    Vinylacetylene aus 1.3-Bis(dialkylamino) -1,3-diethoxyallenen und Alkylidenmalonylchloriden. Kristall-und Molekülstruktur von 3-(Diphenyl)methylen-6-diisopropylamino-5-diisopropyIaminocarbonyl- 2.4-dioxo-3,4-dihydro-2H-pyran [1] Vinylacetylenes from l,3-Bis(dialkylamino)-l,3-diethoxyallenes and Alkylidenemalonyl Chlorides. Crystal and Molecular Structure of 3-(Diphenyl)methylene-6-diisopropylamino-5-diisopropylaminocarbonyl- 2,4-dioxo-3,4-dihydro-2H-pyrane [1]  
  Reference    (Z. Naturforsch. 42b, 97—100 [1987]; eingegangen am 14. Juli 1986) 
  Published    1987 
  Keywords    Tetra Donor Substituted Allenes, Vinylacetylenes, 3-Methylene-2, 4-dioxo-3, 4-dihydro-2H-pyranes, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0097.pdf 
 Identifier    ZNB-1987-42b-0097 
 Volume    42 
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