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1989 (14)
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    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1483.pdf 
 Identifier    ZNB-1989-44b-1483 
 Volume    44 
3Author    Peter Behrens, Mehdi Alidoosti, Frank Schulz, Wolfgang MetzRequires cookie*
 Title    Synthese und Struktur von Graphit-Einlagerungsverbindungen des Quecksilber(II)-chlorids Synthesis and Structure of the G raphite Intercalation Compounds of Mercuric Chloride  
 Abstract    Graphite intercalation com pounds (G IC s) o f mercuric chloride have been synthesized by four different methods: via the vapour phase, from melts o f pure H gCl2. from melts of HgCL and alkali metal chlorides, and from solutions in concentrated aqueous HC1. Com pounds of stages 4, 3 and 2 were obtained, respectively. GICs prepared from solution always show staging disorder. Pure stage com pounds of stage three and four exhibit the follow ing repeat distances along the c axis: c(3) = 1632 pm; c(4) = 1968 pm. Further structural analysis is hindered by the disorder phenom ena common to GICs. Rather surprisingly, m onochrom atic Laue photographs probing the in-plane order o f the intercalate reveal that — regardless o f the preparation method — the diffraction patterns of all com pounds are identical. The main phase possesses a monoclinic in-plane lattice with cell dimensions: a — 390(4) pm , b = 412(4) pm, y — 108.6(3)°. A structure which resembles certain features o f the structure o f pristine HgCL is proposed for this phase. A nother unidentified phase seem s to stabilize this structure in spite o f different amounts o f chlorine excess probably occurring in com pounds prepared in different ways. 
  Reference    Z. Naturforsch. 44b, 721 (1989); eingegangen am 20. Februar 1989 
  Published    1989 
  Keywords    Graphite Intercalation Com pounds Intercalation, HgCL, Structure, Synthesis 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0721.pdf 
 Identifier    ZNB-1989-44b-0721 
 Volume    44 
4Author    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 
5Author    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 
6Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1377.pdf 
 Identifier    ZNB-1989-44b-1377 
 Volume    44 
7Author    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 
8Author    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 
9Author    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 
10Author    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 
11Author    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 
12Author    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 
13Author    Wolfgang Einholz, Gerhard Frey, Wolfgang HauboldRequires cookie*
 Title    Borylierung von Sulfamiden, Sulfoniminen und Sulfondiiminen Borylation of Sulfamides, Sulfonimines and Sulfonediimines  
 Abstract    The diborylated sulfamide 6a can be obtained from 2-chloro-l ,3-dim ethyl-l .3.2-diazaborolidine and the silylated sulfamide la , whereas (M e2N)2BCl and la yield the dithia-tetrazadiborocine 7b. Similarly, (M e2N)2BCl reacts with a) the sulfonimine 2a, b) the sul-fonediim ine 3a to give a) B (N M e:), and the bis-and tris(sulfonim ino)boranes 10b and 11, b) B (N M e2)3 and the dithiatetrazadiborocine 15b. The diborylated sulfamide 6c (R 2B = Ph:B) cannot be isolated. The synthesis of the m onoborylated sulfonim ines 9c, 9e and sulfonediim ines 13, 14 is described. 
  Reference    (Z. Naturforsch. 44b, 47 [1989]; eingegangen am 13. Septem ber 1988) 
  Published    1989 
  Keywords    Boron-Nitrogen Com pounds, Borylated Sulfam ides, Sulfonim ines, Sulfonediim ines, Synthesis, Spectroscopic Data 
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 Identifier    ZNB-1989-44b-0047 
 Volume    44 
14Author    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