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'Crystal Structure' in keywords Facet   section ZfN Section B:Volume 040  [X]
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1985 (34)
1Author    Synthesis, Crystal Structure Of, HerbertW. Roesky, Hartmut Hofmann, Mathias Noltemeyer, GeorgeM. SheldrickRequires cookie*
 Title    Synthese und Kristallstruktur von l,l,l,3,3»3-Hexafluor-2-propylamino- l-thiooxamid +-Hexafluoro-2-propylamino- 1-thiooxamide"  
 Abstract    Dithiooxamide 1 reacts with hexafluoroacetone 2 at room temperature to yield 1,1,1,3,3,3-hexafluoro-2-propylamino-l-thiooxamide 3 and sulfur. The modes of formation of the bis(trifluoromethyl)-methyl group from hexafluoroacetone, the migra-tion of oxygen and the elimination of sulfur are not clear. Crystals of 3 are monoclinic, space group Cc, with a = 2865.3(13), b = 924.4(9), c = 702.9(6) pm, ß = 93.3(7)°. The structure was re-fined to R — 0.067 from 614 reflections. 
  Reference    (Z. Naturforsch. 40b, 124—126 [1985]; eingegangen am 13. August 1984) 
  Published    1985 
  Keywords    Dithiooxamide, Hexafluoroacetone, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0124_n.pdf 
 Identifier    ZNB-1985-40b-0124_n 
 Volume    40 
2Author    KurtO. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von Tl 2 TiS 4 : Ein Perthiotitanat(IV) mit i-[TiS 4 2 "]-Ketten Preparation and Crystal Structure of Tl 2 TiS 4 : A Perthiotitanate(IV) with ^-[TiS 4 2 ~]-Chains  
 Abstract    Tl 2 TiS 4 is orthorhombic, space group Pbca, with a = 22.176(7), b = 9.484(4), c = 6.3977(9) A, Z = 8. The crystal structure was solved by direct methods and refined to a conventional R of0.058 for 704 reflections with I^3a(I). The crystal structure is characterized by infinite perthioanions, i-[TiS 4/2 (S 2) 2 -], which are separated by Tl + -cations. The anion chains are built up by distorted octahedra which share two skew edges to form infinite cis-chains running along [001], The two unshared S-atoms of each octahedron are connected via a S —S-single bond of 2.10 A length. The crystal structure is described as a mixed packing of TI-and S-atoms, composed of puckered T1S 2 -layers, in which the Ti-atoms occupy the octahedral interstices. The relationship of the ^-[XiS^ -]-chains to the anionic groups of Cs 2 TiS 3 is discussed. 
  Reference    Z. Naturforsch. 40b, 229—234 (1985); eingegangen am 27. September 1984 
  Published    1985 
  Keywords    Thallium Perthiotitanate, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0229.pdf 
 Identifier    ZNB-1985-40b-0229 
 Volume    40 
3Author    HerbertW. Roesky, KaveripatnamS. Dhathathreyan, Mathias Noltemeyer, GeorgeM. SheldrickRequires cookie*
 Title    Reactions of the Hexafluorothioacetone Dimer with Cyanides of Phosphorus, Arsenic and Germanium  
 Abstract    Cyanides such as P(CN) 3 , As(CN) 3 , PhP(CN) 2 , Bu'As(CN) 2 and Ge(CN) 4 react with [(CF 3) 2 CS] 2 (1) by insertion of the carbon atom of the /so-nitrile isomer into the four-mem-bered [CS] 2 ring to give compounds PR 3 (2), AsR 3 (3), FP(S)R 2 (4), PhP(S)R^ (5), Bu'AsR^ (6) and GeR 4 (7) respectively, where R' is the novel heterocyclic ligand —N=C—S—C(CF 3) 2 —S —C(CF 3) 2 . The crystal structures of 3 and 7 are reported. 
  Reference    Z. Naturforsch. 40b, 240—246 (1985); received September 19/October 25 1984 
  Published    1985 
  Keywords    Crystal Structure, Hexafluorothioacetone, Nitriles, Heterocyclics 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0240.pdf 
 Identifier    ZNB-1985-40b-0240 
 Volume    40 
4Author    PeterG. Jones, HerbertW. Roesky, Hansjörg Grützmacher, GeorgeM. SheldrickRequires cookie*
 Title    Oxidative Knüpfung einer Phosphor-Phosphor-Bindung unter Einwirkung von Ag(I)-bzw. Cu(II)-Ionen: Synthese und Struktur von [(C 6 H5)PH 2 Ag{|i-(C 6 H 5 PH) 2 }]2 (AsF 6 ) 2 , einem sechsgliedrigen Silber-Phosphor-Ring The Oxidative Formation of a Phosphorus-Phosphorus Bond in the Presence of Ag(I) and Cu(II) Ions: Synthesis and Structure of [(C 6 H 5 )PH 2 Ag{^-(C 6 H 5 PH) 2 }] 2 (AsF 6 ) 2 , Containing a Six-Membered Silver-Phosphorus Ring  
 Abstract    The reaction between AgAsF 6 and phenylphosphine proceeds with formation of a phosphorus-phosphorus bond. The main product 1, [(C 6 H 5)PH 2 Ag{u-(C 6 H 5 PH) 2 }] 2 (AsF 6) 2 , was characterized by an X-ray structure determination [PI, a = 919.0(4), b = 1109.8(4), c = 1316.4(5) pm, a = 97.48(3), ß = 107.25(3), y = 102.71(3)°, Z = 1, R = 0.057 for 2806 observed reflections], 1 contains Ag 2 P 4 rings; the silver atoms are further coordinated by phenylphosphine ligands, thus acquiring trigonal coordination geometry. A similar reaction is observed with Cu(AsF 6) 2 , forming the analogous Cu(I) complex 2. 
  Reference    Z. Naturforsch. 40b, 590—593 (1985); eingegangen am 28. Januar 1985 
  Published    1985 
  Keywords    Crystal Structure, Silver, Phenylphosphine, Copper 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0590.pdf 
 Identifier    ZNB-1985-40b-0590 
 Volume    40 
5Author    G. Erhard, C. Ordier, H. Erbert Schäfer, Michael StelterRequires cookie*
 Title    CanInSb9, eine Zintlphase mit diskreten InSb49 -Anionen On C anInSb9, a New Zintlphase with Discrete InSb49-Anions  
 Abstract    CauInSb9 crystallizes in the orthorhombic system, space group Iba2 (No. 45), with a = 1189.4(5) pm, b = 1259.4(5) pm, c = 1673.0(7) pm. In the structure there are different kinds o f anions, i.e. isolated Sb3~ anions, Sb24~ dumbbells and isolated InSb49* tetrahedra. The new compound belongs to the Zintlphases. 
  Reference    Z. Naturforsch. 40b, 868—871 (1985); eingegangen am 3. April 1985 
  Published    1985 
  Keywords    Calciumantimonidoindate, Crystal Structure, Zintlphase 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0868.pdf 
 Identifier    ZNB-1985-40b-0868 
 Volume    40 
6Author    H. Eribert, W. Adle, Kurt Dehnicke, D. Ieter FenskeRequires cookie*
 Title    (AsPh4)4[CrCl4(/J-N2S2)]4 * 8 CH2C12; Synthese, IR-Spektrum und Kristallstruktur (A sPh4)4[CrCl4(w-N2S2)]4 -8 CH 2C12; Synthesis, IR Spectrum and Crystal Structure  
 Abstract    Trithiazylchloride, (NSC1)3, reacts with metallic chrom ium, with chromium hexacarbonyl, with CrCl3-3 thf, as well as with chrom ium (VI) oxide to form mixtures, in which S4N 3®[CrCl4(N 2S2) ] 0 can be identified as the major product. This com pound reacts with tetraphenylarsonium chloride in dichlorom ethane to form the title com pound, which we have characterized by IR spectroscopy and an X-ray crystal structural analysis. (A sP h4)4[CrCl4(N 2S2)]4 -8 C H 2C12 crystallizes m onoclini-cally in the space group C 2 /c with four formula units per unit cell and with the follow ing lattice constants at —100 °C: a = 2146, b = 2033, c = 3137 pm; ß = 96.0° (9918 independent observed reflexions, R = 0.064). The com pound consists o f A sPh4® ions, tetrameric anions [CrCl4(N 2S2)]44e and included C H 2C12 m olecules. The chromium atom s of the anions occupy the corners o f a nearly ideal square; they are connected via the N -atom s o f planar N 2S2-rings, which are oriented perpendicularly to the Cr4-plane. The chromium atom s com plete their distorted octahedral coordination with four terminal chlorine atom s, the axial ones o f which form short Cl---S-contacts o f average 310 pm to the S-atom s o f the N 2S2-rings. 
  Reference    Z. Naturforsch. 40b, 1314—1319 (1985); eingegangen am 2. Mai 1985 
  Published    1985 
  Keywords    Trithiazylchloride, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1314.pdf 
 Identifier    ZNB-1985-40b-1314 
 Volume    40 
7Author    Rolf Minkwitz, Klaus Jänichen, Herbert Prenzel, Volker WölfelRequires cookie*
 Title    Beiträge zur Chemie der Schwefelhalogenide, 6 [1] Untersuchungen an Trichlorsulfonium(IV)-Salzen Contributions to the Chemistry of Sulfur Halides, 6 [1] Investigations on Trichlorosulfonium(IV) Salts  
 Abstract    The crystal structure of SCl 3 + AsF 6 ~ is reported. The mean S-Cl stretching frequency v of the SC1 3 + cations, weighted according to the degree of degeneration, in the different SC1 3 + X~ salts is directly proportional to the mean S-Cl distance r scl , the force constant f sci and the sulfur.. .anion distance (C1 3 S + .. .X"). That SC1 3 + C1" should be isostructural with PC1 4 ~, the large variation in the S-Cl stretching frequencies in the SC1 3 + X~ salts is due to cation-anion interaction forces. 
  Reference    (Z. Naturforsch. 40b, 53—56 [1985]; eingegangen am 4. Juli/10. Oktober 1984) 
  Published    1985 
  Keywords    Crystal Structure, Bonding and Force Constants, Sulfur Halides 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0053.pdf 
 Identifier    ZNB-1985-40b-0053 
 Volume    40 
8Author    Manfred Regitz, Klaus Urgast, Gerhard MaasRequires cookie*
 Title    Phosphorverbindungen ungewöhnlicher Koordination, 3 [1] Vergleich des Cycloadditonsverhaltens von Diphenylketen und Triphenylphosphen Phosphorus Compounds with Unusual Coordination, 3 [1] Comparison of the Cycloaddition Behaviour of Diphenylketene and Triphenylphosphene  
 Abstract    Triphenylphosphene (3b), generated thermally or photochemically from lb, undergoes olefi-nation reaction with 4.5-benzotropone (6) to yield l-(diphenylmethylen)-4.5-benzocyclohepta-triene (9); the oxaphosphetane 7b is assumed to be the intermediate of this reaction. In an analogous way, 4-pyrone (15) is transformed into 4-(diphenylmethylen)pyrane (16). Correspon-ding olefination behaviour is observed in the reactions of 6 and 15 with diphenylketene. In the reaction of tetracyclone (20) with diphenylketene (3a), the olefination sequence leads to the formation of (diphenylmethylen)tetraphenylcyclopentadiene (21) via betain 22a and the cycloadduct 23a. The spirocyclic reaction product 26a probably arises from the same betain — like intermediate (22 a —> 25 a —> 26 a). The analogy in triphenylphosphene reactivity towards 20 is restricted to the [2+8]-cycloaddition step (formation of 26b). 
  Reference    (Z. Naturforsch. 40b, 67—76 [1985]; eingegangen am 19. Juli 1984) 
  Published    1985 
  Keywords    Diphenylketene, Triphenylphosphene, Cycloaddition with CO-Compounds, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0067.pdf 
 Identifier    ZNB-1985-40b-0067 
 Volume    40 
9Author    Siegfried Pohl, Wolfgang Saak, Bernt KrebsRequires cookie*
 Title    Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX 4 2- (X = CI, Br, I) Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX 4 2 ~ Ions (X = CI, Br, I)  
 Abstract    The compounds [(C 6 H 5) 4 As] 2 TeCl 4 (1), [(C 2 H 5) 4 N] 2 TeBr 4 • CH 3 CN (2), and [(C 2 H 5) 4 N] 2 TeI 4 (3) were prepared by the reaction of Te, X 2 , and excess (QH^NX (X = Br, I) in acetonitrile solution or by heating of [(C 6 H 5) 4 As] 2 TeCl 6 , Te, and (C 6 H 5) 4 ASC1 for several hours in the same solvent. The structures of 1—3 were determined from single crystal X-ray data. 1 crystallizes in the monoclinic space group P2 x ln with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, ß = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, 14/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te —CI, Te —Br, and Te—I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively. 
  Reference    Z. Naturforsch. 40b, 251—257 (1985); eingegangen am 22. Oktober 1984 
  Published    1985 
  Keywords    Tetrahalotellurates(II), Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0251.pdf 
 Identifier    ZNB-1985-40b-0251 
 Volume    40 
10Author    Udo Demant, Elke Conradi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure  
 Abstract    [HC(NH 2) 2 ] 3 FeCl 6 was obtained together with other products from the reaction of S 4 N 4 with HCl in H 2 CC1 2 in the presence of FeCl 3 . Its crystal structure was determined from X-ray diffraction data (473 in-dependent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c — 876.4 pm; tetragonal, space group P4 2 /m, Z = 2. Of the two crystallo-graphically independent formamidinium ions HC(NH 2) 2 ®, one exhibits positional disorder; the other one has C—N bond lengths of 128 pm. The FeCl 6 30 ions have symmetry C 2h , but the deviation from O h is small. 
  Reference    Z. Naturforsch. 40b, 443—445 (1985); eingegangen am 6. November 1984 
  Published    1985 
  Keywords    Formamidinium-Hexachloroferrate(III), Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0443_n.pdf 
 Identifier    ZNB-1985-40b-0443_n 
 Volume    40 
11Author    Heinz Hoberg, Klaus Radine, Carl Krüger, MariaJ. RomãoRequires cookie*
 Title    Synthese neuer Phosphan-Nickel(I)-KompIexe und Kristallstruktur von /# 3 Jodo-fra-^-iodo-cycIotris(triphenylphosphan-nickel), (TPP) 3 Ni 3 I 4 Synthesis of New Phosphine Nickel(I) Complexes and Crystal Structure of // 3 -Iodo-m's-//-iodo-cyclotris(triphenylphosphine Nickel), (TPP) 3 Ni 3 I 4  
 Abstract    Synthesis and properties of the new nickel(I) complexes (COD)Ni(TPP)I (3) and (TCP)Nil (5) are reported. Reaction of 3 and 5 with diphenylacetylene (7) yields alkyne complexes (R 3 P)NiI(PhC2Ph)Ni(R 3 P)I (R = Ph (8a), and Cy (8b)). In solution, 3 disproportionates to give nickel(O) and (TPP) 3 Ni 3 I 4 (12)), the structure of which has been determined by X-ray crystallogra-phy. Cluster compound 12 is cleaved into monomeric units by addition of ligands such as TPP or CO (TPP = triphenylphosphine, TCP = tricyclohexylphosphine, COD = 1,5-cyclooctadiene). 
  Reference    Z. Naturforsch. 40b, 607—614 (1985); eingegangen am 17. Januar 1985 
  Published    1985 
  Keywords    Nickel(I), Alkyne Complex, Cluster, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0607.pdf 
 Identifier    ZNB-1985-40b-0607 
 Volume    40 
12Author    Ulrich Schwanitz-Schüller, Arndt SimonRequires cookie*
 Title    Synthese und Kristallstruktur von Gd 2 NCl 3 Synthesis and Crystal Structure of Gd 2 NCl 3  
 Abstract    The new compound Gd 2 NCl 3 is formed from GdCl 3 with Gd and N 2 as well as from GdCl 3 with GdN (at 1020 K). The crystal structure contains NGd 4 tetrahedra, which are linked via opposite edges to form infinite chains (Orthorhombic, Pbcn; a = 1301.7(1), b = 673.10(6), c = 614.03(7) pm; R = 0.031 for 578 independent reflections). The formal analogy with structures containing condensed clusters, e.g. Gd 2 Cl 3 , is discussed. 
  Reference    Z. Naturforsch. 40b, 705—709 (1985); eingegangen am 31. Oktober 1984 
  Published    1985 
  Keywords    Rare Earth Nitride Chloride, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0705.pdf 
 Identifier    ZNB-1985-40b-0705 
 Volume    40 
13Author    Horst Sabrowsky, Alfred Thimm, Petra MertensRequires cookie*
 Title    Kaliumlithiumsulfid, KLiS: Das erste Interalkalimetallsulfid Potassium Lithium Sulphide, KLiS: The First Inter Alkaline Metal Sulphide  
 Abstract    The compound KLiS has been prepared and its crystal structure is determined by X-ray dif-fraction techniques. The hygroscopic, yellow compound crystallizes in the tetragonal space group P4/nmm (Z = 2) with the cell parameters a — 431.79(4), c = 696.20(9) pm. The structure was solved from 2100 counter reflections (356 symmetry independent reflections) through a Patterson synthesis and refinement by Fourier syntheses to a least squares residue of 0.026. The structure is characterized by c-centered squares of lithium layers interspersed by anti-parallel ordered K—S-pairs forming an anti-PbFCl-type geometry. 
  Reference    Z. Naturforsch. 40b, 733—735 (1985); eingegangen am 8. Februar 1985 
  Published    1985 
  Keywords    Potassium Lithium Sulphide, Crystal Structure, X-Ray 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0733.pdf 
 Identifier    ZNB-1985-40b-0733 
 Volume    40 
14Author    Jens Anhaus, ZafarA. Siddiqi, HerbertW. Roesky, JanW. Bats, Yalcin ElermanRequires cookie*
 Title    Reaktion von Tetraschwefeltetranitrid mit Rhenium(VII)-chloronitrid Die Kristallstruktur von [Ph 4 As + ] 2 [Cl 4 Re(NS)(NSCl) 2_ ] * CH 2 C1 2 Reaction of Tetrasulfurtetranitride with Rhenium(VII)-chloronitride The Crystal Structure of [Ph 4 As + ] 2 [Cl 4 Re(NS)(NSCl) 2_ ] * CH 2 C1 2  
 Abstract    The synthesis of [Ph 4 As + ] 2 [Cl 4 Re(NS)(NSCl) 2 ~] • CH 2 C1 2 (4) from the reaction of S 4 N 4 , Cl 4 ReN, and Ph 4 AsCl is reported. CH 2 C1 2 is used as solvent. The reaction of S 4 N 4 with Re 2 Cl 10 similarly leads to the salt [Ph 4 As + ][Cl 5 ReNS~] (5) in a smaller yield. 4 crystallizes in the triclinic space group PI with Z -2, a = 10.434(2), b = 12.1454(6), c -21.125(2) Ä, a = 81.210(6), ß = 86.70(1), Y = 76.624(8)°. 
  Reference    Z. Naturforsch. 40b, 740—744 (1985); eingegangen am 6. Februar 1985 
  Published    1985 
  Keywords    Thionitrosyl Complexes, Rhenium(VII), Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0740.pdf 
 Identifier    ZNB-1985-40b-0740 
 Volume    40 
15Author    KurtO. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von Na4GeSe4: Ein neues orr/io-Selenogermanat(IV) Preparation and Crystal Structure of Na4GeSe4: A New 0 rt/20-Selen0 germ anate(IV )  
 Abstract    Na4GeSe4 was obtained from a stoichiometric melt of Na2Se, Ge and Se at 750 °C. It crystallizes with a new orthorhombic structure, space group Pnma, with a = 28.518(8), b — 9.447(5), c = 7.128(2) Ä , Z = 8 . The crystal structure was refined to a conventional R of 0.074 for 1236 reflections with I > 3 a (I) (diffractometer data). It is characterized by discrete GeSe44"-anions with almost regular tetrahedral geometry. Two independent anions appear in the structure, the mean Ge — Se-bond lengths are 2.345 and 2.353 Ä, resp. The Na+-ions are coordinated to 4 —6 chalco-gen atoms in the range 2.88—3.28 Ä. The structure is composed of mixed cation-anion-slabs, 2 [Na2(G eSe4)2_], which run parallel to the bc-plane and are separated from each other by corrugated 36-layers of N a+-ions. 
  Reference    Z. Naturforsch. 40b, 878 (1985); eingegangen am 25. März 1985 
  Published    1985 
  Keywords    Sodium Selenogermanate(IV), Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0878.pdf 
 Identifier    ZNB-1985-40b-0878 
 Volume    40 
16Author    Wolfgang Jeitschko, ElkeJ. ReinboldRequires cookie*
 Title    Strukturchemische Untersuchungen an Scandium-Cobalt-Phosphiden mit einem Metall:Phosphor-Verhältnis von 2:1  
 Abstract    Several new scandium cobalt phosphides were prepared by reaction of the elemental compo­ nents in a tin flux. ScCoP has a TiNiSi-type structure with the orthorhombic lattice constants a = 6.268(2) Ä , b = 3.750(1) Ä , c = 7.050(3) Ä. ScCo5P3 is isotypic with YCo5P3. Its orthorhom­ bic lattice constants are: a = 11.691(5) Ä , b = 3.583(1) A, c = 10.206(3) Ä. Sc2C o12P7crystallizes with the hexagonal Zr2F e12P7 structure with a = 8.973(3) A , c = 3.531(1) Ä. Sc5C o19P12 is of a new type which is closely related to the structure of Hf2Co4P3. It has hexagonal symmetry, space group P 62m —D 3h and the lattice constants a -12.124(7) Ä , c = 3.633(2) Ä , with Z = 1 formula unit per cell. The structure was determined and refined with isotropic thermal parameters from single-crystal counter data to a residual of R = 0.023 for 848 unique structure factors and 24 variable parameters. Considering the environments of the phosphorus atoms the structures are all closely related. There are, however, considerable differences in the coordination polyhedra of the metal atoms. 
  Reference    Z. Naturforsch. 40b, 900—905 (1985); eingegangen am 26. März 1985 
  Published    1985 
  Keywords    Tin Flux, Crystal Structure, Scandium Cobalt Phosphides 
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 Identifier    ZNB-1985-40b-0900 
 Volume    40 
17Author    Thomas Godemeyer, Alexander Berg, Hans-Dieter Groß, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    ji-Nitridokomplexe von Wolfram(VI) Die Kristallstruktur von PPh4[W2NCl10] /<-Nitrido Complexes of Tungsten(VI) The Crystal Structure of PPh4[W2NCl10]  
 Abstract    W2NC19 was obtained as a brilliant red crystal powder from tungsten hexachloride and tris(trim ethylsilyl)am ine. A ccording to its IR spectrum it has dimeric m olecules [W 2NC19]2 with bridging chlorine atom s. Its reaction with tetraphenylphosphonium chloride yields PPh4[W2N C l10], and with phosphorus oxide chloride W 2NCl9 O PCl3 is obtained; both are soluble in dichlorom ethane. The crystal structure of PPh4[W2N C l10] was determined_ by X-ray diffraction (2521 observed reflexions. R = 0.065). Crystal data: triclinic, space group P I , Z = 2, a = 1125.7, b — 1278.2, c = 1347.8 pm, a = 110.08, ß = 94.55, y = 111.55°. The structure consists o f PPh4® ions which are arranged to (PPh4®)2 pairs about inversion centres, and o f [W2N C l10]e anions. The latter possess an alm ost linear W NW group (173°) with slightly different WN bond lengths o f 179 and 188 pm corresponding to double bonds. Each tungsten atom has an octahedral coordination. The WC1 bonds trans to the nitrido ligand are about 9 pm longer than the bonds in the cis positions. 2. Synthesen und IR-Spektren der /i-Nitridokomplexe W2NC19 erhält man gemäß Gl. (1) durch Um set­ zung von Wolframhexachlorid mit Tristrimethylsilyl-amin in Trimethylchlorsilan als Lösungsmittel: 2 WC16 + N(SiMe3) 3 < 9 °C> W2NC19 + 3 Me3SiCl (1) Zur Herstellung eines reinen Produktes hat sich die Anwendung von Trimethylchlorsilan, in dem sich WC16 beträchtlich löst, als ebenso bedeutsam erwie­ sen wie die Kühlung des Reaktionsansatzes < 9 °C. Erhöht man die Temperatur, so findet bereits bei 20 °C langsam und ausschließlich die Bildung des auch auf andere Weise zugänglichen WNC13 [1] statt. Wählt man in diesem Fall das Mengenverhältnis der Reaktanden nach (1), so läßt sich schließlich die Hälfte des WC16 zurückgewinnen. Bei Anwendung molarer Mengen 1:1 erhält man direkt reines WNC13: WC16 + N(SiM e3) 3 2 0 °C > WNC13 + 3 Me3SiCl (2) Für den Mechanismus der Reaktion (1) nehmen wir einen stufenweisen Verlauf an, bei dem sukzessive Trimethylchlorsilan abgespalten wird. Erstes mögli­ ches Zwischenprodukt wäre dann Cl5WN(SiMe3)2, das wir allerdings nicht isolieren konnten. Die A b­ spaltung eines zweiten Trimethylchlorsilans führt 0 ® dann zur Bildung des Imids C14W =N —SiMe3, das 
  Reference    Z. Naturforsch. 40b, 999—1004 (1985); eingegangen am 4. April 1985 
  Published    1985 
  Keywords    «-Nitrido C om plexes Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0999.pdf 
 Identifier    ZNB-1985-40b-0999 
 Volume    40 
18Author    Hans Hartl, Irene Brüdgam, F. Mahdjour-Hassan-AbadiRequires cookie*
 Title    Synthese und Strukturuntersuchungen von Iodocupraten(I) VI. Iodocuprate(I) mit zweikernigen Anionen [CU2I4]2-und [Cu2I6]4-[1] Syntheses and Structure Analyses of Iodocuprates(I) VI. Iodocuprates(I) with Dinuclear Anions [Cu2I4]2-and [Cu2I6]4-[1]  
 Abstract    Bis(dipyridiniom ethan)-di-,a-iodotetraiododicuprate(I), [Py2CH 2]2[Cu2I6] and two m odifica­ tions o f bis(tetraphenylphosphonium)-di-^-iodo-diiododicuprate(I) were obtained by reacting Cu with I2 and [Py2C H 2]I2 or [PPh4]I in acetone. The crystal structures o f these com pounds are built up by the cations and the binuclear anions: edge sharing C ul4-tetrahedra in [Cu2I6]4~ and edge sharing, nearly trigonal planar C u l3-units in [Cu2I4]2~. W hereas the Cu2I4 anions (-A) are centrosym m etric and almost planar, the anions (-B) are folded about the bridging I---I contact. The anions [Cu2I6] are in intimate contact with the I -C interactions. 
  Reference    Z. Naturforsch. 40b, 1032—1039 (1985); eingegangen am 1. April 1985 
  Published    1985 
  Keywords    Iodocuprates(I), Synthesis, Crystal Structures 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1032.pdf 
 Identifier    ZNB-1985-40b-1032 
 Volume    40 
19Author    Giuliano Bandoli, KurtJ. Irgolic, Antonio Grassi, GiuseppeC. PappalardoRequires cookie*
 Title    Solid State and Solution Conformation of Di-2-thienyl Telluride: X-Ray Structure and Dipole Moment Studies  
 Abstract    The crystal and m olecular structure of di-2-thienyl telluride was determ ined by X-ray analysis. 
  Reference    Z. Naturforsch. 40b, 1157—1160 (1985); received April 1 1985 
  Published    1985 
  Keywords    Di-2-thienyl Telluride, X-Ray, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1157.pdf 
 Identifier    ZNB-1985-40b-1157 
 Volume    40 
20Author    Brigitte Eisenmann, Hanna Jordan, Herbert SchäferRequires cookie*
 Title    Ba2Sb3, eine neue Zintlphase mit Sb6-Ketten On Ba2Sb3, a N ew Zintl Phase with Sb6-Chains  
 Abstract    The new com pound Ba2Sb3 crystallizes in the monoclinic system, space group P2[/c (No. 14) with the lattice constants a = 693.4(3) pm , b = 1345.3(6) pm , c = 1581.7(6) pm, ß = 90.25(15)°. The compound is isotypic to the Sr2Sb3 structure with discrete Sb68-chain anions. 
  Reference    Z. Naturforsch. 40b, 1603 (1985); eingegangen am 17. Juli 1985 
  Published    1985 
  Keywords    Barium A ntim onide, Crystal Structure, Zintl Phase 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1603.pdf 
 Identifier    ZNB-1985-40b-1603 
 Volume    40 
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