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'Crystal Structure' in keywords Facet   section ZfN Section B:Volume 038  [X]
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1983 (34)
1Author    HeinzDieter Lutz, Willi Buchmeier, Bernward EngelenRequires cookie*
 Title    Crystal Structure of Lead Sulfite  
 Abstract    The crystal structure of orthorhombic PbSOß (Pnma, Z = 4, a = 790.3(1), b = 548.8(1), c = 680.2(1) pm) has been determined using single crystal X-ray diffraction data (final R for 663 reflections with I > 2<r(I) = 0.052). The para-meters of the atoms in the asymmetric unit are: Pb(4c) 0.. The sulfite ion has S-O distances of 149.4(7) and 153.7(5) (twice) pm. The Pb-0 distances of the edge-connected Pb-0 7 polyhedra (distorted mono-capped trigonal prism) range from 253.4(5) to 284.8(5) pm. The structure is closely related to that of PbS04. 
  Reference    Z. Naturforsch. 38b, 523—525 (1983); eingegangen am 16. Dezember 1982 
  Published    1983 
  Keywords    Lead Sulfite, Crystal Structure, Sulfite 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0523_n.pdf 
 Identifier    ZNB-1983-38b-0523_n 
 Volume    38 
2Author    Karl-Friedrich Tebbe, Roland FröhlichRequires cookie*
 Title    Untersuchungen an Polypseudohalogeniden, II [1] Darstellung und Kristallstruktur des Rubidiumdicyanotriiodids, Rb[I(ICN)2] Preparation and Crystal Structure of Rb[I(ICN)2]  
 Abstract    The new compound Rb[I(ICN)2] can be prepared in aqueous solution by simple addition of two mole equivalents of ICN to one formula unit Rbl. The solid is isotypic with CS[I(ICN)2] and crystallizes in the orthorhombic space group Pmmn with a = 16.246 A, b = 6.795 A, c = 4.397 A and Z = 2. The crystal structure has been solved from diffracto-meter data and refined to R = 0.035 for 313 observed reflections. The structure may be interpreted as a layer-like package of Rb+ cations and pentahalide-analogous anions [I(ICN2]~. The anionic groups are angular with symmetry mm 2 and y(I-I--I) = 128.69°, 0>(I--I-C) = 175.5°, <p(I-C-N) = 177°, d(I~-I) = 3.271 A, d(I-C) = 2.11 A, d(C-N) = 1.13 A. The cation is surrounded by a distorted cube of iodine atoms with a minimum distance d(Rb-I) = 3.775 Ä. Some additional results on the reactions of alkali halides and halogenocyans in different solvents are mentioned and compared with those described elsewhere. 
  Reference    Z. Naturforsch. 38b, 549—553 (1983); eingegangen am 14. Februar 1983 
  Published    1983 
  Keywords    Rubidiumdicyanotriiodide, Polypseudohalide, Pseudopentahalide, Crystal Structure 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0549.pdf 
 Identifier    ZNB-1983-38b-0549 
 Volume    38 
3Author    Wilhelm Isenberg, NaylaK. Homsy, Jens Anhaus, HerbertW. Roesky, GeorgeM. SheldrickRequires cookie*
 Title    Synthese und Struktur von N2S3C1 + SbCI^ Synthesis and Structure of N2S3C1+ SbCl6~  
 Abstract    N2S3C1+ SbClö -was prepared by chlorination of N4S4 • SbCls with elemental chlorine. The crystals are monoclinic, P2i/c, with a = 1492.4(4), b = 1233.6(2), c = 1437.5(4) pm, ß = 91.40(2)°, and R = 0.059 for 3663 observed reflections. There are two independent cations and anions in the asymmetric symmetric unit. The appreciable interionic inter-action results in a high density of q = 2.642 g • cm -3 (calcd). In einer vorausgegangenen Arbeit berichteten wir u.a. über Reaktionen des Chlortrithiadiazylchlorids 1 mit Lewis-Säuren [1], Bei diesen Reaktionen wird im allgemeinen nur das ionogen gebundene Cl sub-stituiert, so daß sich Verbindungen der Formel N2S3C1+ MCI4-(M = AI, Fe) ergeben. Lediglich SbCls reagiert mit 1 unter Substitution beider Cl zu N2S3(SbCle)2. Die Bildung der monosubstituierten Verbindung N2S3C1+ SbCls -2 wurde nicht beob-achtet. Nun gelang uns die Darstellung von 2 durch Chlorierung des Addukts N4S4 • SbCls [2] mit ele-mentarem Chlor. Experimenteller Teil 
  Reference    Z. Naturforsch. 38b, 808—810 (1983); eingegangen am 25. März 1983 
  Published    1983 
  Keywords    Chlorotrithiadiazol, Hexachloroantimonate, Crystal Structure 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0808.pdf 
 Identifier    ZNB-1983-38b-0808 
 Volume    38 
4Author    Walter AbrielRequires cookie*
 Title    Die Kristallstruktur von [Na(H20)3]2TeBr6, ein Hydrat mit Ketten aus flächenkondensierten Na(H20)6-Oktaedern The Crystal Structure of [Na(H20)3]2TeBr6, a Hydrate with Chains of Face-Sharing Na(H20)6 Octahedra  
 Abstract    Using 293 K diffractometer intensity data the structure of [Na(H20)3]2TeBr6 has been determined by single crystal X-ray technique and refined to a final Rw of 0.048. The crystals are monoclinic (space group C2/m) with a — 13.039(4) A, b = 10.899(8) A, c = 6.838(3) A, ß = 115.89(2)° and Z = 2. The structure contains infinite chains parallel [001] built up by face-sharing Na(H20)6-octahedra. Isolated TeBrß 2-octahedra between these chains represent the anion part of the structure, which can be regarded as a packing of layers based on a 3 3 .4 2 .-net consisting of oxygen and bromine atoms. 
  Reference    Z. Naturforsch. 38b, 1543—1547 (1983); eingegangen am 20. Juli 1983 
  Published    1983 
  Keywords    Crystal Structure, Hydrates, Tellurates 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-1543.pdf 
 Identifier    ZNB-1983-38b-1543 
 Volume    38 
5Author    Annegret LipkaRequires cookie*
 Title    Darstellung und Kristallstruktur des 2:3-Adduktes von Antimontrichlorid und 4-Phenylpyridin, 2 SbCl3 * 3 (CnH9N) Preparation and Crystal Structure of the 2:3 Adduct of Antimony Trichloride and 4-Phenylpyridine, 2SbCl3 * 3(CnH9N)  
 Abstract    A congruently melting phase of molar ratio 2:3 was identified in the system SbCl3/4-phenylpyridine. The structure consists of two different types of complex units: One SbCl3 molecule is bonded to one 4-phenylpyridine ligand only, whereas the other one forms a complex with two 4-phenylpyridine ligands. The SbCl3 unit in the 1:1 species is pyrami-dally shaped, whereas the SbCl3 unit in the 1:2 species displays a T-shaped geometry. The mean angle between the phenyl and pyridyl planes is 33.3°; mean bond lengths are <Sb-Cl> = 247.6 pm and <Sb-N> = 241.7 pm. 
  Reference    Z. Naturforsch. 38b, 341—346 (1983); eingegangen am 27. September 1982 
  Published    1983 
  Keywords    Antimony Trichloride, Crystal Structure, Stereochemistry 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0341.pdf 
 Identifier    ZNB-1983-38b-0341 
 Volume    38 
6Author    Brigitte Eisenmann, Hanna Jordan, Herbert SchäferRequires cookie*
 Title    Preparation and Crystal Structure of Ba6Sn2P6  
 Abstract    The new compound BaeSn2P6 crystallizes in the monoclinic system, space group P2i/c with lattice constants a = 883.7 ± 0.5 pm b = 1268.8 ± 0.8 pm c= 862.3 ± 0.5 pm ß = 114.42 ± 0.10°. The compound is isotypic to KeSn2Te6 and contains the Sn2P6 12_ -anions which are isosteric with the Sn2Te6 6_ -units. 
  Reference    Z. Naturforsch. 38b, 404—406 (1983); eingegangen am 4. November 1982 
  Published    1983 
  Keywords    Bariumhexaphosphidohypodistannate, Zintl Phase, Crystal Structure 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0404_n.pdf 
 Identifier    ZNB-1983-38b-0404_n 
 Volume    38 
7Author    Achim Müller, Winfried Hellmann, Uwe Schimanski, Rainer Jostes, WilliamE. NewtonRequires cookie*
 Title    On the Central Role of Sulfur in Multi Metal Aggregates with Different Electron Populations: [S2WS2CoS2WS2]' 1 - (n -2, 3)  
 Abstract    The hetero metal sulfur aggregates [Co(WS4)2] n ~ (with variable electron popula-tion: n = 2, 3) could be isolated as salts and characterized by physical measurements (in-cluding X-ray structure analysis). Experimental and theoretical investigations show that due to a strong metal -> ligand electron delocalisation WS4 2-(like M0S4 2 -) is a non-innocent ligand and that the additional charge upon reduction is located mainly at the S atoms of the ligand system. 
  Reference    Z. Naturforsch. 38b, 528—529 (1983); eingegangen am 12. November 1982 
  Published    1983 
  Keywords    Preparation, Crystal Structure, Molecular Structure, Electronic Structure, Thioanions 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0528_n.pdf 
 Identifier    ZNB-1983-38b-0528_n 
 Volume    38 
8Author    Ulrich Müller, Paul KlingelhöferRequires cookie*
 Title    /3-NbBr5, eine neue Modifikation von Niobpentabromid mit einer eindimensionalen Lagenfehlordnung ß-NbBrs, a New Modification of Niobium Pentabromide Having One-Dimensional Stacking Disorder  
 Abstract    While trying to react NbBrs with sulfur in a closed tube, crystals of the new modification /?-NbBra were obtained. Its X-ray diffraction patterns have sharp reflexions and diffuse streaks showing the presence of a one-dimensional disorder. From the sharp reflexions alone, a statistically averaged sub-structure results; it has the space group Ccmm and the lattice constants ao = 644, bo = 1867 and Co = 615 pm. Taking into account the diffuse streaks, the true structure was deduced; its lattice constants are a = 2ao, c = Co, b indefinite due to the disorder. /?-NbBrs is isostructural to tantalum pentaiodide. It consists of layers of (NbBrs)2 molecules that are stacked with displacement faults in the direction of b. The bromine atoms have a hexagonal close-packing arrangement. 
  Reference    Z. Naturforsch. 38b, 559—561 (1983); eingegangen am 25. Januar 1983 
  Published    1983 
  Keywords    Niobium Pentabromide, Crystal Structure, Stacking Faults 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0559.pdf 
 Identifier    ZNB-1983-38b-0559 
 Volume    38 
9Author    Gerhard Thiele, Kurt WittmannRequires cookie*
 Title    Über Hydraziniumsalze von Iodoplatinaten On Hydrazinium Salts of Iodoplatinates  
 Abstract    The new compounds (N2H5)2Ptl6 and (^Hs^Ptls • H2O were obtained by reaction of H2PtCl6 with N2H5CI and HI in aqueous solutions. In the crystal structure of the ortho -rhombic bis[hydrazinium(+I)]hexaiodoplatinate(IV) (^Hs^Ptle the N2H5+ cations and Ptlö 2-anions build up a K^PtClß-like arrangement. Bis[hydrazinium(+I)]pentaiodo-platinate(II,IV)hydrate, (N2Hs)2Ptl5 • H20, is classed with the group of linear chain mixed-valence platinum complexes which have highly anisotropic properties. In the crystal structure are structurally undistinguishable Ptl4-units (Pt-I = 264 pm) connected by asymmetric I-bridges (Pt-I = 270 pm and 338 pm) to 1 [Ptl4l2/2] chains. 
  Reference    Z. Naturforsch. 38b, 674—679 (1983); eingegangen am 15. Februar 1983 
  Published    1983 
  Keywords    Iodoplatinates, Hydrazinium Salt, Mixed-Valence Compound, Crystal Structure 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0674.pdf 
 Identifier    ZNB-1983-38b-0674 
 Volume    38 
10Author    H.-J Kraus, H. Werner, C. KrügerRequires cookie*
 Title    Synthese und Struktur von C5Me5Pd(PR3)X: Palladiumkomplexe mit einem unsymmetrisch gebundenen Pentamethylcyclopentadienylring [ 1 ] Synthesis and Structure of CsMe5Pd(PR3)X: Palladium Complexes with an Unsymmetrically Bonded Pentamethylcyclopentadienyl Ring [1]  
 Abstract    The complexes C5Me5Pd(PR3)X (1-4) are prepared from [Cl(PR3)Pd]2(iM-OCOCH3)2 and TICsMes. Attempts to replace the halide ligand by a second CsMes or a C5H5 unit remained unsuccessful. The X-ray structure analysis of C5MesPd[P(i-Pr)3]Cl (3) indicates that the five-membered ring shows a tendency of »^-bonding towards the metal. Das Interesse an Pentamethylcyclopentadienyl-metall-Verbindungen ist in den letzten Jahren stän-dig gestiegen, nachdem an zahlreichen Beispielen gezeigt werden konnte, daß die Einführung des CsMes-an Stelle des CsHs-Liganden eine Zunahme der Stabilität der Ring-Metall-Bindung bewirkt [2], In der Reihe der Platinmetalle sind Komplexe mit CsMes vor allem von Rhodium und Iridium darge-stellt und auch strukturell charakterisiert worden; die Arbeiten von P. M. Maitlis und seiner Gruppe haben hier bahnbrechend gewirkt [3]. Im Vergleich dazu ist nur relativ wenig über Pentamethylcyclopentadienylpalladium-Verbindun-gen bekannt. Wir hatten kürzlich gefunden [4], daß bei der Umsetzung der Acetat-verbrückten Zwei-kernkomplexe [Cl(PR3)Pd]2(//-OCOCH3)2 mitTICsHö die Verbindungen (^ 5 -C5H5)Pd(?? 1 -C5H5)PR3 entste-hen, die in Lösung ein fluktuierendes Verhalten zei-gen. Aufgrund von !H-und 13 C-NMR-spektrosko-pischen Messungen sind zwei dynamische Prozesse nachweisbar, wobei der Prozeß mit der größeren Aktivierungsenergie ein nja-(bzw. rf/r] 1 -)-Aus-tausch der beiden unterschiedlich gebundenen Cy-clopentadienylliganden und derjenige mit der kleine-ren Altivierungsenergie eine metallotrope Umlage-rung ist. Die Koaleszenztemperatur für den 
  Reference    Z. Naturforsch. 38b, 733—737 (1983); eingegangen am 1. März 1983 
  Published    1983 
  Keywords    Pentamethylcyclopentadienylpalladium Complexes, Synthesis, Crystal Structure, Bonding Mode 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0733.pdf 
 Identifier    ZNB-1983-38b-0733 
 Volume    38 
11Author    Roland Schmidt, Wolfgang Hiller, Gerhardt PausewangRequires cookie*
 Title    Peroxofluorokomplexe der Übergangsmetalle, V [1-3]  
 Abstract    Kristallstruktur von K2Ti(02)F4 • H20 (orange) mit einem Di(/i-fluoro)diperoxo-hexafluorodititanat(IV)-Anion Transition Metal Peroxofluoro Complexes, V [1-3] Crystal Structure of K2Ti(02)F4 • HcO (orange) with a Di(J«-fluoro)diperoxo-hexafluorodititanate(IV) Anion Orange crystals of K2Ti(02)F4 ' H20 have been obtained from aqueous solution. The crystal structure (space group P2i/n, a = 604.3(3), b = 1424.6(4), c = 761.0(2) pm, ß = 103.98°, Z = 4, dc = 2.63 gem-3 , dm = 2.62 gem-3 , R = 0.051 for 2257 independent reflections) shows isolated di(ja-fluoro)-bridged [Ti2(02)2Fg] 4 -anions, which are inter-connected by hydrogen bonded H20 forming infinite chains. 
  Reference    Z. Naturforsch. 38b, 849—851 (1983); eingegangen am 17. März 1983 
  Published    1983 
  Keywords    K2Ti(02)F4 @BULLET H20, Crystal Structure, Preparation, Properties 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0849.pdf 
 Identifier    ZNB-1983-38b-0849 
 Volume    38 
12Author    Brigitte Eisenmann, Herbert Schäfer, Heike SchrodRequires cookie*
 Title    Über das o-Natriumtelhirostannat(rV) Na4SnTe4 On the o-Sodium-tellurostannate(IV), Na4SnTe4  
 Abstract    The new compound Na4SnTe4 crystallizes in the orthorhombic system, space group P2i2i2i with lattice constants a = 865.8(5) pm, 6 = 884.0(5) pm, and c = 1526.9(8) pm. In the structure there are isolated SnTe4 4 ~-tetrahedra. In seinen binären Chalkogenverbindungen tritt das Zinn gegenüber 0, S und Se in den beiden Oxi-aationsstufen 11+ und IV + auf, während mit Tellur bisher nur das SnTe charakterisiert werden konnte. Auch in ternären Telluriden ist mit Aus-nahme des AggSnTee [1, 2] und des K2SnTe5 [3] Zinn in der Oxidationsstufe IV+ gegenüber Tellur unbekannt. Es überrascht daher, daß sich die Ver-bindung Na4SnTe4, wie wir jetzt fanden, in glatter Reaktion aus den Elementen synthetisieren läßt. Darstellung Zur Darstellung wurden die Elemente in stöchio-metrischen Anteilen unter feuchtigkeits-und sauer-stofffreier Argonatmosphäre in eine bei 150 °C vor-getrocknete Quarzampulle eingewogen. Dabei mußte das Natrium, um den Verlust durch die Reaktion mit dem Gefäßmaterial auszugleichen, nach empi-rischem Befund im Überschuß von ca. 15 Gew.-% zugesetzt werden. Die Ampullen wurden eva-kuiert, abgeschmolzen und in mit Argon gefüllten 
  Reference    Z. Naturforsch. 38b, 921—923 (1983); eingegangen am 17. Mai 1983 
  Published    1983 
  Keywords    o-Sodiumtellurostannate(IV), Preparation, Crystal Structure 
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 Identifier    ZNB-1983-38b-0921 
 Volume    38 
13Author    Ali Mahan, Albrecht MewisRequires cookie*
 Title    A B2X2 -Verbindungen mit CaAl2Si2-Struktur, IX [1] Compounds with the CaAl2Si2 Structure, IX [1]  
 Abstract    The compounds ZrCu2P2, YZnCuP2, LaZnCuP2, and CeZnCuP2 have been prepared and their structures have been determined. They are isotypic and crystallize trigonally in the CaAl2Si2-type structure (space group P3m 1) with the lattice constants: ZrCu2P2 a = 381,2(1) pm, c = 617,1(2) pm, YZnCuP2 a = 398,3(1) pm, c = 652,3(2) pm, LaZnCuP2 a = 408,2(1) pm, c = 674,2(2) pm, CeZnCuP2 a = 406,4(1) pm, c = 669,7(2) pm. 
  Reference    Z. Naturforsch. 38b, 1041—1045 (1983); eingegangen am 13. Mai 1983 
  Published    1983 
  Keywords    Ternary and Quaternary Phosphides, Copper, Zinc, Crystal Structure 
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 Identifier    ZNB-1983-38b-1041 
 Volume    38 
14Author    Sigurd Elz, Armin Buschauer, Martin Dräger, Walter SchunackRequires cookie*
 Title    Darstellung, Eigenschaften und Kristallstruktur der N-[2-(4.5.6.7-Tetrahydro-2-benzimidazolyl)-ethyl] -phthalamidsäure Preparation, Properties and Crystal Structure of N-[2-(4.5.6.7-Tetrahydro-2-benzimidazolyl)-ethyl]-phthalamic Acid  
 Abstract    During syntheses using the phthalimide rest in liquid, ethanolic or aqueous ammonia, phthalamides, phthalimides or phthalamic acids are formed depending on reaction condi-tions and work-up. As demonstrated by the synthesis of the title compound via hydrolysis of 4 with aqueous ammonia, dipolar ions of phthalamic acids are obtained if the phthal-imide-N substituent is sufficiently basic. The crystal structure of 5 • 4H2O has been determined and refined until R = 0.0878. It shows a vast system of hydrogen bonds. 
  Reference    Z. Naturforsch. 38b, 1203—1207 (1983); eingegangen am 3. Juni 1983 
  Published    1983 
  Keywords    Crystal Structure, Phthalamic Acid, Phthalamide, Phthalimide 
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 Identifier    ZNB-1983-38b-1203 
 Volume    38 
15Author    Bernhard Lippert, Helmut Schöllhorn, Ulf ThewaltRequires cookie*
 Title    Platin in seiner ungewöhnlichen Oxidationsstufe —III: Diplatin(III)-Komplexe der Modellnukleobase 1-Methyluracil Platinum in its Unusual Oxidation State -fill: Diplatinum(III) Complexes with the Model Nucleobase 1-Methyluracil  
 Abstract    Oxidation of the head-tail dimer cis-[(NH3)2Pt(l-MeU)]2(N03)2 (1-MeU = 1-methyl-uracilato anion, C5H5N2O2) with a mixture of nitrous and nitric acid yields three crystalline 
  Reference    Z. Naturforsch. 38b, 1441—1445 (1983); eingegangen am 15. Juli 1983 
  Published    1983 
  Keywords    Diplatinum(III), Crystal Structure, 1-Methyluracil Complex 
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 Identifier    ZNB-1983-38b-1441 
 Volume    38 
16Author    Hubert Schmidbaur, Beatrix Milewski-Mahrla, FritzE. WagnerRequires cookie*
 Title    Synthese, Struktur und Sb-Mößbauer-Spektren kovalenter und ionischer Tetraorganoantimon(V) -Verbindungen Synthesis, Structure and Sb-Mößbauer Spectra of Covalent and Ionic Tetraorganoantimony(V) Compounds  
 Abstract    Tetramethylstibonium and tetraphenylstibonium oxinate*(l, 2) and anthranilate (4, 5) have been prepared from the antimony pentaorganyls and 8-oxy-quinoline or anthranilic acid, respectively. The crystal structure determination of 1 revealed covalent molecules with planar bidentate oxinate as part of a distorted coordination octahedron at antimony. -121 Sb-Mößbauer spectra of 1, 2, 4, 5 and of tetramethylstibonium acetylacetonate (3) are also in agreement with covalent structures, but a pentacoordinate environment of Sb is more likely for the anthranilates 4, 5. The spectra of the hydrogendicarboxylates 6-9, however, point to ionic stuctures with, if any, only weak donor interactions of the anions with the stibonium cations. 
  Reference    Z. Naturforsch. 38b, 1477—1483 (1983); eingegangen am 14. Juli 1983 
  Published    1983 
  Keywords    Organoantimony Compounds, Mößbauer Spectra, Crystal Structure 
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 Identifier    ZNB-1983-38b-1477 
 Volume    38 
17Author    Siegfried PohlRequires cookie*
 Title    Synthesis and Crystal Structure of a Polymeric Adduct of 2,2'-Dipyridil and Iodine: CioHgN^  
 Abstract    The reaction of 2,2'-dipyridil with iodine (I2; molar ratio 1:3) in CH2C12 solution yields the polymeric complex 2,2'-dipyridil(I2)3. The crystal structure of the compound was determined from single crystal X-ray data (monoclinic, C2/c, a — 3215.0(16), b = 439.9(1), c = 1824.1(9) pm, ß = 130.79(3)°, Z = 4). 2,2'-Dipyridil(I2)3 forms infinite chains of alternating Iß units and bifunctional dipyri-dil molecules. 
  Reference    Z. Naturforsch. 38b, 1535—1538 (1983); eingegangen am 12. Juli 1983 
  Published    1983 
  Keywords    2, 2'-Dipyridil(I2)3, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-1535.pdf 
 Identifier    ZNB-1983-38b-1535 
 Volume    38 
18Author    Uwe Klingebiel, Norbert Vater, William Clegg, Martin Haase, GeorgeM. SheldrickRequires cookie*
 Title    Synthesis of Silicon-Phosphorus-Rings - Structure of a cis-2,2,4,4-Tetrakis(silylamino)-l,3-diphospha-2,4-disilacyclobutane  
 Abstract    Fluorosilylphosphanes of the type R2SiFPHR' (R = CHMe2, CMe3, NMeSiMe3; R' = H, C6H5; 1-4) are obtained in the reaction of difluorosilanes with lithiated phosphanes in a molar ratio 1:1. Diphosphasilanes (5, 6) and a difluorosilylphosphane (7) are isolated as by-products. 1-4 react with w-QjHgLi to give cyclic silylphosphanes, LiF, and C4H10 (8-11). Dilithiated 5 reacts with F2PN(CMe3)SiMe3 to form of a four-membered SiP3-ring 12. The 31 P NMR spectra of 9 and 11 show signal coalescence for the eis-and tfrans-isomers at room temperature. The crystal structure of the cis-isomer of 11 has been determined. The substituted ring 13 is prepared in the reaction of lithiated 9 and Me2SiF2. 
  Reference    Z. Naturforsch. 38b, 1557—1562 (1983); eingegangen am 6. Juli 1983 
  Published    1983 
  Keywords    Fluorosilylphosphanes, Cyclisation, P-Inversion, Isomers, Crystal Structure 
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 Identifier    ZNB-1983-38b-1557 
 Volume    38 
19Author    Rüdiger Kniep, Lutz Körte, Dietrich MootzRequires cookie*
 Title    Kristallstrukturell von Verbindungen A2X2 (A = S, Se; X = Cl, Br) Crystal Structures of Compounds A2X2 (A = S, Se; X = Cl, Br)  
 Abstract    The crystal structures of compounds A2X2 (A = S, Se; X = Cl, Br) contain molecules X-A-A-X with dihedral angles between 83.9° and 87.4°. Three different types of molecular packing are realized: S2CI2, S2Br2 (a-Se2Br2) and /?-Se2Br2(Se2Cl2). Details of molecular geometries as well as crystal structures are discussed. 
  Reference    (Z. Naturforsch. 38b, 1—6 [1983]; eingegangen am 20. August 1982) 
  Published    1983 
  Keywords    Sulfur(I) Halides, Selenium(I) Halides, Crystal Structure 
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 Identifier    ZNB-1983-38b-0001 
 Volume    38 
20Author    Kurt Klepp, Weif BrongerRequires cookie*
 Title    Na6CoS4 -ein Thiocobaltat mit isolierten CoS4-Anionen Na6CoS4 -A Thiocobaltate with Isolated C0S4 Anions  
 Abstract    NaeCoS4 crystallizes in the hexagonal space group P 63111c with a —890.9(2) pm and c = 687.8(2) pm, Z = 2. The crystal structure was determined from four circle diffracto-meter data and refined to a conventional .ff-value of 0.020. NaöCoS4 is isotypic with NaeZnC>4. The crystal structure can be derived from a h.c.p. arrangement of S atoms. Co atoms occupy tetrahedral voids, the resulting CoS4-tetrahedra being almost regular with an average Co-S distance of 235 pm. Na atoms occupy tetrahedral and octahedral voids in the ratio 1:1. 
  Reference    (Z. Naturforsch. 38b, 12—15 [1983]; eingegangen am 27. August 1982) 
  Published    1983 
  Keywords    Crystal Structure, Ternary Chalcogenides, Cobalt Compounds 
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 Identifier    ZNB-1983-38b-0012 
 Volume    38 
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