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'Crystal Structure' in keywords Facet   section ZfN Section B:Volume 044  [X]
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1989 (26)
1Author    Petra Krieger-Beck, A. Ndreas Brodbeck, Joachim SträhleRequires cookie*
 Title    Synthesis and Structure of K2A u3, a New Phase in the System Potassium —Gold  
 Abstract    K2A u 3 is obtained from the elem ents in a sealed Ta am poule as air-sensitive needles with a golden lustre. It crystallizes in the orthorhom bic space 
  Reference    Z. Naturforsch. 44b, 237—239 (1989); eingegangen am 18. O ktober 1988 
  Published    1989 
  Keywords    Dipotassium Triauride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-0237_n 
 Volume    44 
2Author    Brigitte Eisenmann, Roland ZaglerRequires cookie*
 Title    Selenoantimonate  
 Abstract    (V): Darstellung und Struktur von Na3SbSe4, K3SbSe4 und [Ba(en)4]2[Ba(en)3](SbSe4)2 Selenoantim onates(V): Preparation and Crystal Structure of N a3SbSe4, K3SbSe4 and [Ba(en)4]2[Ba(en)3](SbSe4) 2 The crystal structures of N a 3SbSe4, K3SbSe4 and [B a(en)4]2[B a(en)3](SbSe4)2 contain isolated tetrahedral anions SbSe43 -, which are the first exam ples o f selenoantim onates(V). Na3SbSe4 
  Reference    Z. Naturforsch. 44b, 249 (1989); eingegangen am 24. Oktober 1988 
  Published    1989 
  Keywords    Selenoantim onates, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0249.pdf 
 Identifier    ZNB-1989-44b-0249 
 Volume    44 
3Author    HansG. Eorg Stammler, Johannes WeissRequires cookie*
 Title    Synthese  
 Abstract    und Kristallstruktur von (S4N3)2Se2Cl10, (S4N3)2Se2CI6 und [(S4N3)SeCl5]n Synthesis and Crystal Structure of (S4N3)2Se2C l10, (S4N3)2Se2Cl6, and [(S4N 3)SeCl5]" (S4N 3)2S e2C l10, (S4N 3)2Se2Clft and [(S4N 3)SeC l5]" are formed by the reaction o f S4N 4, Se2Cl2, and SO C l2. The structures o f the three com pounds where determ ined by X-ray diffraction. The yellow crystals o f (S4N 3)2Se2C l10 are monoclinic, space group P 2,/a, a = 817.5(2) pm , b = 1790.4(5) pm, c = 843.1(6) pm, ß = 104.31(4)°, Z = 2. The Se2C l102~ anion consists o f 2 Cl-bridged distorted octahedra. (S4N 3)2Se2Cl6 forms red m onoclinic crystals, space group P2,/c, a = 1036.5(3) pm , b = 1376.5(5) pm , c = 1400.4(4) pm ,/3 = 100.65(2)°, Z = 4. In the Se2Cl62" anion the Se atoms have a square planar environm ent. The yellow crystals o f (S4N 3)SeC l5 are orthorhom bic, space group P 2 12 12 1, a = 734.2(3) pm , b — 989.4(4) pm , c = 1627.4(6) pm , Z = 4. In the SeC l5_ anion the Se atom has an octahedral environm ent o f chlorine atom s, thus forming a polym eric structure. 
  Reference    Z. Naturforsch. 44b, 1483 (1989); eingegangen am 5. Mai 1989 
  Published    1989 
  Keywords    Thiotrithiazyl-chloroselenates, Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-1483 
 Volume    44 
4Author    Dieter Schmidt-Bäse, Uwe KlingebielRequires cookie*
 Title    Von 1,5-funktionelIen Trisiloxanen zu (SiO)4-, [Si(OSiN)2Si]-und [0 (S i0 S i)2N]-Ringen From 1,5-Functional Trisiloxanes to (SiO)4-, [Si(OSiN)2Si]-, and [0(Si0Si)2N]-Rings  
 Abstract    C om pounds of the general formula (CM e3)2Si(R)O H , (R = Cl, O H . N H :) react with «-C 4H,,Li or Na to give the alkali silanolates 1—5 .1 —5 serve as starting materials in the reactionsw ithchlorosilanes for the synthesis o f siloxanes (6—12). Ring closure reactions of dilithiated 9 ,1 1 , and 12 occur with SiCl4 (13) and C l,SiM e, (15, 16). 13 contains an (SiO)4. 15 an Si(O SiN),Si. and 16 an 0 (S i0 S i) ,N eight-m em bered ring. Hydrolysis o f 13 leads to the formation o f the hydroxy-substituted eight-m em bered ring 14. The crystal structures of (C M e3),S i(O H) —O —SiM e, —Ö —(H ,N)S i(C M e3), (11) and M e,Si[O Si(C M e3),N H ],S iM e, (15) are reported and discussed. 
  Reference    Z. Naturforsch. 44b, 395 (1989); eingegangen am 16. D ezem ber 1988/23. Januar 1989 
  Published    1989 
  Keywords    Silanolates, Siloxanes, Am inosiloxanol Eight-M embered Rings, Crystal Structure 
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 Identifier    ZNB-1989-44b-0395 
 Volume    44 
5Author    W. S. Sheldrick, H. G. BraunbeckRequires cookie*
 Title    Preparation and Crystal Structure of Cs4Sn2Se6  
  Reference    Z. Naturforsch. 44b, 851 (1989); eingegangen am 8. Februar 1989 
  Published    1989 
  Keywords    Cesium Selenostannate(IV ), M ethanolotherm al Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0851_n.pdf 
 Identifier    ZNB-1989-44b-0851_n 
 Volume    44 
6Author    Hans Hartl, Irene BrüdgamRequires cookie*
 Title    Synthese und Strukturuntersuchungen von Iodocupraten(I)  
 Abstract    X . [Co(cp)2]2[CuI3] und [Co(cp)2][Cu2I3] = l/9{[Co(cp)2]9[Cu6Iu Ji [(Cn6I8)2]} [ 1 ] Syntheses and Structure Analyses of Iodocuprates(I) X. [Co(cp)2]2[CuI3] and [Co(cp)2][Cu2I3] = l/9{[Co(cp)2]9[Cu6I n]2[(Cu6I8)2]} [1] Bis-(cobalticenium)triiodocuprate(I), [ C o (c p) 2]2[ C u I , ] s (l) and cobalticenium-triiodo-dicuprate(I), [Co(cp)2][Cu2I,]=l/9{[Co(cp)2]9[Cu6I u ] 2 [(Cu6I8)2]}==(2) were obtained by reacting [Co(cp)2]I with Cul in acetone 1 and acetonitrile 2, respectively. The crystal structure of 1 exists of cobalticenium cations and mononuclear planar anions C u l,2". The crystal structure of 2 contains cobalticenium cations and two different types of iodocuprate(I) anions: an isolated hexa-nuclear ion Cu6I n5-built up by 6 edge sharing C ul4 tetrahedra and polymeric layers 2 [CuftI8]2-. In the latter anion Cu6I n components are two-dimensionally connected via 3 common edges and Cu(I) ions are distributed over two kinds of tetrahedral sites. 
  Reference    Z. Naturforsch. 44b, 936—941 (1989); eingegangen am 10. März/28. April 1989 
  Published    1989 
  Keywords    Iodocuprate(I), Cobalticenium Cation, Crystal Structure, Synthesis 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0936.pdf 
 Identifier    ZNB-1989-44b-0936 
 Volume    44 
7Author    Tetraphenylphosphonium Hexachlorodizincate, Hexachlorodicadmate, JörgH. Ubertus, Wilhelm, Ulrich MüllerRequires cookie*
 Title    Tetraphenylphosphonium-hexachlorodizinkat und -hexachlorodicadmat, (PPh4)2Zn2CI6 und (PPh4)2Cd2Cl6  
 Abstract    The title com pounds were obtained by the reactions of PPh4Cl. HC1 and ZnS or CdS in C H 2C12. Their crystal structures were determ ined by X-ray diffraction. (PPh4),Z n,C l6: a = 973.6(1), b = 982.6(2), c = 1296.7(3) pm, a = 107.93(2), ß = 94.50(2), y = 100.91(2)°, R = 0.036 for 2237 unique observed reflexions. (PPh4)2Cd2Cl6: a = 977.1(2), b = 997.5(3). c = 1306.6(3) pm. a = 108.81(2), ß = 94.18(2), y = 100.24(2)°, R = 0.050 for 1921 reflexions. Both com pounds are isotypic in the triclinic space group P I and consist of PPh4 ions and dimeric, centrosymm etric M2Clg-ions in which the tetrahedrally coordinated metal atoms are linked via chloro bridges. Synthese von (PPh4)2Zn2Cl6 und (PPh4)2Cd2CI6 
  Reference    Z. Naturforsch. 44b, 1037—1040 (1989); eingegangen am 26. April 1989 
  Published    1989 
  Keywords    H exachlorodizincate, H exachlorodicadm ate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-1037 
 Volume    44 
8Author    Z. NaturforschRequires cookie*
 Title    Stereoselective Synthesis o f a Phenylphosphido-Bridged Dimetallic Complex: Crystal and Molecular Structure of [(R * ,R * ),(R * )]-(± )-[(i/5-C5H 5){l,2 -C 6H 4(PM ePh)2}FePH Ph{Cr(CO )5}]- 2 H20 * 0.5 CH2C12 * 0.5 C4H 80  
 Abstract    D eprotonation of (R * ,R *)-(±)-[(^ -C 5H 5){l,2-C 6H 4(PM ePh)2}Fe(PH 2Ph)]PF6 with «-BuLi in tetrahydrofuran at 20 °C, followed by treatm ent of the interm ediate phenylphosphido-iron complex with [Cr(CO)5(NM e3)] produces a separable 3 :2 mixture of the diastereom ers [(R* ,R*),(R*)]-and [(R*,R*),(S*)]-(±)-'[(/75-C5H 5){ l,2 -C 6H 4(PM ePh)2} F e -P H (P h) -*■ C r(C O)5], The m ajor com po­ nent of the mixture crystallizes from dichlorom ethane-tetrahydrofuran in the atm osphere as the mixed solvate [(R *,R *),(R *)]-(±)-[(/75-C5H 5){ l,2 -C 6H 4(PM ePh)2} F e -P H (P h) -* C r(C O)5]-2 H 20 0.5C H iC l2-0.5 C 4H 80 in the triclinic space group P I with two formula units in the unit cell; the lattice constants are a = 10.933(2) Ä , b = 13.161(4) Ä ,c = 15.249(3) A, a = 76.83(1)°, 0 = 75.62(3)°, and y = 79.31(1)°. In the structure, the pyram idal phenylphosphido group bridges the dissimilar metals via relatively long m etal-phosphorus bonds, v iz., Fe —P = 2.285(5) Ä, C r—P = 2.511(4) Ä. 
  Reference    Z. Naturforsch. 44b, 1041 (1989); received M arch 29 1989 
  Published    1989 
  Keywords    Stereoselective Synthesis, Dimetallic, Bridging Phenylphosphido, Crystal Structure 
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 Identifier    ZNB-1989-44b-1041 
 Volume    44 
9Author    Reiner Figge, Claus Friebel, U. Te Patt-Siebel, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Nitridokomplexe von Molybdän(V); Synthesen, IR-und EPR-Spektren. Die Kristallstruktur von [Na(15-Krone-5)Na(THF)]2[MoNCI3 THF]4-2THF Nitrido Complexes of M olybdenum (V ); Syntheses, IR , and EPR Spectra. Crystal Structure of [N a(15-Crow n-5)N a(TH F)]2[MoNCl3-THF]4-2T H F  
 Abstract    Nitrido C om plexes o f M olyb denu m (V), 
  Reference    Z. Naturforsch. 44b, 1377—1384 (1989); eingegangen am 30. Mai 1989 
  Published    1989 
  Keywords    Syntheses, IR Spectra, EPR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-1377 
 Volume    44 
10Author    W. S. Sheldrick, H. G. BraunbeckRequires cookie*
 Title    Preparation and Crystal Structure of Cs4Se16  
 Abstract    The cesium polyselenide Cs4 S e 16 has been prepared by the m ethanolotherm al reaction o f Cs2 C 0 3 and Se at 160 °C and 13 bar. [S e16]4-fragments may be regarded as containing an Se6 ring with Cs symmetry and two Se5 chains related by the crystallographic mirror plane. S e4 o f the six-m em bered ring, which displays a square planar geom etry, participates in two relatively long S e 4 —Se5 bonds [2.989(4) A ] to individual chains. The /rans-sited S e 4 —Se3 bonds [2.425(4) Ä] are markedly longer than the remaining S e -S e bonds in the Se6 ring [2.344(4), 2.356(4) Ä ]. Further Se —Se interactions o f length 3.132(4) and 3.346(4) Ä are observed betw een individual [Sel6]4~ fragments. 
  Reference    Z. Naturforsch. 44b, 1397—1401 (1989); eingegangen am 26. Mai 1989 
  Published    1989 
  Keywords    Cesium P olyselenide, M ethanolotherm al Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-1397 
 Volume    44 
11Author    JörnM. Üller, Corinna Hänsch, Joachim PickardtRequires cookie*
 Title    ;r-01efin-Iridium-Komplexe, XV [1] Kationische Bis(2.3-dimethylbutadien)iridium-L-Verbindungen mit verschiedenen Donorliganden L jr-Olefin Iridium Complexes, XV [1] Cationic Bis(2.3-dim ethylbutadiene)iridium-L Compounds with Various D onor Ligands L  
 Abstract    (dm b)2IrCH , (dm b = 2.3-dim ethylbuta-l,3-diene) reacts with Ph,CBF4 in C H 2C12 to form the 
  Reference    Z. Naturforsch. 44b, 278 (1989); eingegangen am 10. Oktober 1988 
  Published    1989 
  Keywords    Synthesis, IR Spectra, NM R Spectra, Mass Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-0278 
 Volume    44 
12Author    Karl-Friedrich Tebbe, N. Orbert KraußRequires cookie*
 Title    Untersuchungen an Polypseudohalogeniden, VI [1] Darstellung und Kristallstruktur des Natriumdicyanoiodat(I)-dihydrats, Na[I(CN)2] * 2 H20 Studies on the Polypseudohalides, VI [1] Preparation and Crystal Structure of N a[I(CN )2] -2 H 20  
 Abstract    The new com pound N a[I(C N)2] • 2 H 20 can be prepared by addition o f iodine to a concentrated aqueous solution of sodium cyanide. It crystallizes in the monoclinic space group P 2,/c with a — 1044.0(2), b — 480.2(2), c = 730.2(2) pm , ß — 95.94(2)° and Z = 2. The crystal structure has been refined to Rf = 0.027 for 692 reflections. The structure may be described as a layer-like package o f cations N a+, water m olecules and trihalide-analogous anions [I(C N)2]~. The anion is strictly linear at the I atom and nearly linear at the C atom s with cp(l—C —N) = 176.2° and d(I —C) = 231.1, d (C —N) = 110.6 pm. The cation is surrounded by a slightly distorted octahedron o f nitrogen and oxygen atoms with d(N a--N) = 263.8, d(N a--O) = 242.0, 242.8 pm. 
  Reference    Z. Naturforsch. 44b, 637 (1989); eingegangen am 27. Januar 1989 
  Published    1989 
  Keywords    Sodium dicyanoiodate, C yanogen Com pound, Polypseudohalide, Pseudotrihalide, Crystal Structure 
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 Identifier    ZNB-1989-44b-0637 
 Volume    44 
13Author    Georg Beuter, Joachim SträhleRequires cookie*
 Title    Clusteraufbau durch Photolyse von R3PAuN3  
 Abstract    , III [1] Synthese von [(Ph3PAu)5Fe(CO)3]PF6 und Ru3(CO)10(jM-AuPPh3)(/i-NCO) Cluster Synthesis by Photolysis of R3PA uN 3, III [1] Synthesis of [(Ph3PA u)5Fe(C O)3]PF6 and R u3(C O)10(«-A uPPh3)(w-NCO) Photolysis of a mixture of Ph3P A u N 3 with F e(C O)5, Fe2(C O)9 or Fe3(C O),2 in TH F yields [(Ph3P A u)5F e(C O)3]+ (1) which crystallizes with PF6" as counterion as air stable, yellow platelets in the space group P2,/c: a = 2230.0(7), b = 1655.0(6), c = 2462.7(8) pm, ß = 94.04(5)°, Z = 4. The cationic A u5Fe cluster forms a bicapped F eA u 3 tetrahedron with almost equal Fe — A u dis­ tances o f 259.0 to 265.1 pm to all five A u atoms. D ue to the local symmetry C3|, o f the F e(C O)3 group two v(CO) at 1880 and 1930 c m ' 1 are observed. C o-photolysis of R u3(C O),2 and Ph3P A uN 3 does not result in a cleavage of the R u3 cluster. Bridging ,w-AuPPh3 and /^-NCO groups substitute two CO ligands to form Ru3(C O)10 («-A uPP h3)(u-N C O) (2). 
  Reference    Z. Naturforsch. 44b, 647 (1989); eingegangen am 26. Januar 1989 
  Published    1989 
  Keywords    Pentagold Iron Cluster, Synthesis, Crystal Structure, Triruthenium M onogold Cluster 
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 Identifier    ZNB-1989-44b-0647 
 Volume    44 
14Author    Kurt Merzweiler, D. Ieter Fenske, Eva Hartm, Ann, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur des Imidokomplexes {TaCl4NC(Ph)[N(SiM e3)2]}2 * 2 C H 2C 12 Synthesis and Crystal Structure of the Imido Complex {TaCl4NC(Ph)[N(SiM e3)2]}2 * 2 C H 2C12  
 Abstract    The title com pound has been prepared by the reaction of N ,N,N '-tris(trim ethylsilyl)benz-amidine with tantalum pentachloride in C H 2CL suspension, forming am ber-coloured, moisture-sensitive crystals, which were characterized by an X-ray structure determ ination. Space group P 2,In, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (— 65 °C): a — 1165.2(6), b -1335.4(6), c = 1629.0(7) pm, ß -93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCLTa with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in frarcs-position to the imido group, which can be formulated a sT * a= $ = C < *M (bond len g th sT a= N = 183.5(8), C = N = 134(1) pm. bond angle TaNC = Ph 162.7(7)°). 
  Reference    Z. Naturforsch. 44b, 1003 (1989); eingegangen am 8. Mai 1989 
  Published    1989 
  Keywords    Imido Complex of Tantalum, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-1003 
 Volume    44 
15Author    Wolfgang Blase, G.Erhard CordierRequires cookie*
 Title    D ie Kristallstruktur von Na3Ga8Sn3 und die Interpretation der Bindungsverhältnisse auf der Basis der Wadeschen Regeln und des Zintlkonzeptes The Crystal Structure of Na3G a8Sn3 and the Interpretation of its Chemical Bonding According to W ade's Rules and the Zintl Concept  
 Abstract    The crystal structure of Na3G a8Sn3 (a = 1532.7(7), b = 890.7(6), c = 1224.9(8) pm; ß = 129.6(2)°, space group C2/m) contains G a l2 icosahedra and puckered layers of condensed six-m em bered Ga/Sn rings, which are interconnected by additional Ga/Sn atoms to a three-dim en­ sional framework. The Na content of the com pound correlates with the num ber of electrons necessary for a stable electron configuration in the anionic partial structure. 
  Reference    Z. Naturforsch. 44b, 1011—1014 (1989); eingegangen am 10. April 1989 
  Published    1989 
  Keywords    Sodium -Gallium -Stannides, Crystal Structure, W ade's Rules, Zintl Concept 
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 Identifier    ZNB-1989-44b-1011 
 Volume    44 
16Author    EvaH. Artm Ann, Kurt Dehnicke, D. Ieter Fenske, Helm Ut Goesmann, G.Erhard BaumRequires cookie*
 Title    [Na-15-Krone-5]2[ZrF2Cl4] und (PPh4)2[ZrCI6] * 2 CH2CI2; Synthesen, IR-Spektren und Kristallstrukturen [Na-15-Crown-5]2[ZrF:Cl4] and (PPh4)2[ZrCl6] * 2 C H 2C12; Syntheses, IR Spectra, and Crystal Structures  
 Abstract    [Na-15-crown-5]: [Z rF2Cl4] has been prepared by the reaction of the amidinato complex [Ph—C(NSiM e3)2Z rC l3]2 with sodium fluoride in acetonitrile suspension, as well as by the reaction ° f Z rC l4 in acetonitrile, both in the presence of 15-crown-5. On an analogous route (PPh4)2[ZrCl6] • 2 CH2C12 has been prepared by the reaction of [P h -C (N S iM e3)2Z rC l3]2 with PPh4Cl in C H 2C12 solution, as well as by the reaction of ZrC l4 with PPh4Cl in C H 2C12. The compounds are characterized by their IR spectra and by crystal structure determ inations. [Na-15-crown-5]2[ZrF2Cl4]: Space group P 2 1/a, Z = 4, 6589 observed independent reflexions, R = 0.069. Lattice dimensions at 20 °C: a = 1705.0(9), b = 1092.4(6), c = 1906.5(10) pm , ß = 113.14(3) . [Na-15-crown-5]2[ZrF2Cl4] forms ion triples, in which both sodium ions are seven-coordinate by five oxygen atoms of the crown ether molecules, as well as by a fluorine and a chlorine atom of the c/s-[ZrF2Cl4]2~ unit. (PPh4)2[ZrCl6] -2 C H 2C12: Space group P I , Z = 1, 4831 observed independent reflexions, R = 0.041. Lattice dimensions at 20 °C: a = 1030.1(5), b = 1124.8(6), c = 1245.6(6) pm, a = 70.81(3), ß = 80.61(4), y = 80.39(4)°. The com pound has an ionic structure with Z rC l62^ ions of symmetry Cr 
  Reference    Z. Naturforsch. 44b, 1155 (1989); eingegangen am 21. Juni 1989 
  Published    1989 
  Keywords    H alogeno-Zirconates(IV ), Syntheses, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-1155 
 Volume    44 
17Author    Klaus Hosier, Frank Weller, Kurt DehnickeRequires cookie*
 Title    Kristallstruktur von [MoC12(N S N )-2TH F]2; einem Metallaheterocyclus mit der NSN4 -Einheit Crystal Structure of [MoC12(N S N )-2T H F ]2; a M etallaheterocycle with the NSN4-Unit  
 Abstract    The chlorothionitrene complex [Cl4M o(NSCl)]2 reacts with N ,N,N '-tris(trim ethylsilyl)benzam idine in T H F solution to form the heterocyclic complex [MoC12(NSN) ■ 2T H F ]2, which contains the [NSN]4-unit. The com pound is characterized by IR spectro­ scopy and by an X-ray structure determ ination (Space group P2,/c, Z = 2, 1504 observed unique re ­ flexions, R = 0.044. Lattice dim ensions at 19 °C: a = 1176.0(1), b = 1108.6(4), c = 1227.3(3) pm, ß = 118.25(1)°). The com pound forms centrosym m etric molecules [(TH F)2C12M o(NSN)2MoC12(T H F)2], in which the molybdenum atoms are members of a nearly planar M o(NSN)2Mo eight-m em bered ring with bond lengths MoN 180.2 and 175.2 pm; NS 157.5 and 160.6 pm; the bond angle NSN is 108.3°, corresponding to a NSN4-unit. 
  Reference    Z. Naturforsch. 44b, 1325—1328 (1989); eingegangen am 5. Juni 1989 
  Published    1989 
  Keywords    M etallaheterocycle with NSN4~ U nit, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-1325_n 
 Volume    44 
18Author    FrankW. Eller, Harald Borgholte, H. Arald Stenger, Stefan Vogler, Kurt DehnickeRequires cookie*
 Title    Synthesen und Kristallstrukturen der Kronenether-Komplexe (18-Krone-6) * 2 CH3CN, [Na-15-Krone-5][Re04] CH3CN und [Na-15-Krone-5]PF6 Syntheses and Crystal Structures of the Crown E ther Complexes (18-C row n-6)-2C H 3CN, [N a-15-Crow n-5][Re04] * C H 3CN, and [Na-15-Crown-5]PF6  
 Abstract    Single crystals o f (18-crow n -6)-2C H 3CN were obtained by cooling a solution o f 18-crown-6 in acetonitrile to 4 °C. Space group P 2 x/n, Z = 2, 629 observed independent reflexions, R = 0.062. Lattice dim ensions at 19 °C: a = 911.7(1), b = 852.0(1), c = 1370.0(2) pm; ß — 104.61(1)°. The com pound forms a m olecular structure with approximate D 3d symmetry o f the crown ether m olecule, and C —H -O interactions of the acetonitrile m olecules with the crown ether, the H ---0 distances being 243, 253, and 267 pm , respectively. [N a-15-crow n-5][R e04] • C H 3CN is formed as a by-product o f the reaction o f R eN C l4 with sodium fluoride in acetonitrile in the presence o f 15-crown-5 and traces o f water. Space group P 1, Z = 2, 3107 observed independent reflexions, R = 0.045. Lattice dim ensions at 19 °C: a — 823.4(1), b = 1078.8(1), c = 1204.0(1) pm; a = 112.40(1)°, ß = 94.35(1)°, y = 104.63(1)°. The com pound forms ion pairs, in which the sodium atom is sixfold coordinated by the five oxygen atoms o f the crown ether m olecule, as well as by one oxygen atom o f the R e 0 4~ ion, which is only slightly distorted. The bond length Na — 0 R e 0 3 is 237.8(8) pm , the bond angle N aO R e is 164.3(5)°. [Na-15-crown-5]PF6 is formed in the reaction o f [R eC l3(N SC l)2 • PO C l3] with sodium fluoride in acetonitrile solution in the presence o f 15-crown-5. Space group P na2,, Z = 4, 1130 observed independent reflexions, R = 0.123. The high R value is due to disorder of the skeletal atoms of the crown ether m olecule. The com pound forms ion pairs, in which the sodium atom is sevenfold coordinated by the five oxygen atom s o f the crown ether m olecule, as well as by two fluorine atom s o f the PF6~ ion with N a —F bond lengths o f 240(2), and 246(2) pm, respectively. 
  Reference    Z. Naturforsch. 44b, 1524 (1989); eingegangen am 25. Juli/5. September 1989 
  Published    1989 
  Keywords    Crown Ether C om plexes, Syntheses, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-1524 
 Volume    44 
19Author    M. Somer, W. Hönle, H. G. Von SchneringRequires cookie*
 Title    Darstellung, Kristallstruktur und Schwingungsspektren von Cs3A s7 und Cs3(NH3)A s7 Syntheses, Crystal Structure and Vibrational Spectra of Cs3As7 and Cs3(NH3)As7  
 Abstract    Cs3A s7, a com pound with cage-like A s73" anions, has been prepared from the elem en ts in sealed quartz am poules at 820 K. The ruby-red com pound undergoes a first order phase transition at 640 K and is obtained as m icrocrystalline samples. The structure o f the low-tem perature a-m odification is not known, but /3-Cs3A s7 belongs to the plastically crystalline ß -R b 3P7 type o f 
  Reference    Z. Naturforsch. 44b, 296 (1989); eingegangen am 15. Novem ber 1988 
  Published    1989 
  Keywords    Tricesium heptaarsenide, Tricesium am m oniateheptaarsenide, Crystal Structure, Vibrational Spectra, H eptaarsanortricyclene Anion 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0296.pdf 
 Identifier    ZNB-1989-44b-0296 
 Volume    44 
20Author    JohnDavid Kildea, Wolfgang Hiller, Beatrice Borgsen, Kurt DehnickeRequires cookie*
 Title    Synthese, IR-Spektrum und Kristallstruktur des Amidinatokomplexes [N a(15-K rone-5)][Ph—C(NSiM e3)2SnCl3F] Synthesis, IR Spectrum, and Crystal Structure of the Amidinato Complex [N a(15-Crow n-5)][Ph-C(N SiM e3)2SnCl3F]  
  Reference    Z. Naturforsch. 44b, 889 (1989); eingegangen am 30. März 1989 
  Published    1989 
  Keywords    N, N '-Bis(trim ethylsilyl)am idinato C om plex, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1989-44b-0889 
 Volume    44 
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