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121Author    Susanne Maier, Wolfgang Hiller, Joachim Strähle, Christina Ergezinger, Kurt DehnickeRequires cookie*
 Title      
 Abstract    The copper(I)amidinato complex Cu 2 [Ph-C(NSiMe 3) 2 ] ; has been prepared by the reaction of CuCl with N.N,N'-tris(trimethylsilyl)benzamidine in boiling acetonitrile. forming white crystals. The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion. Crystal data: space group PI, Z = 2 (2851 observed independent reflexions, R = 0.047). Lattice dimensions at 20 °C: a = 1135.0(3); b = 1219.6(4); c = 1372.4(4) pm; a = 106.74(3)°; ß = 107.92(4)°; y = 91.40(4)°. The compound forms dimeric molecules with a short Cu--Cu contact of 242 pm and two chelating amidinato ligands with Cu-N bond lengths of (averaged) 189.0 pm and bond angles N —C—N of 124.1°. 
  Reference    Z. Naturforsch. 43b, 1628—1632 (1988); eingegangen am 11. August/30. September 1988 
  Published    1988 
  Keywords    Synthesis, X-Ray, Copper(I) Amidinato Complex 
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 Identifier    ZNB-1988-43b-1628 
 Volume    43 
122Author    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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 Identifier    ZNB-1989-44b-0721 
 Volume    44 
123Author    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 
124Author    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 
125Author    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 
126Author    Siegfried PohlRequires cookie*
 Title    Thioharnstoff-Derivate als Liganden in  
 Abstract    Eisen-Komplexen: Synthese und Kristallstrukturen von [FeI2L2l, [Fe2I4L3], (L -L) 2+|FeI4-| 2 (L = (M e2N)2CS) und |Fe2I4(C6H l0(N H -C S -N H M e)2)2| mit einer Notiz zu [FeIL3]+|Fe4S4I3L]-T hiourea D erivatives as Ligands in Iro n Complexes: Syntheses and C rystal Structures o f [F eI2L2], [ F e J 4 L3], (L -L) 2 +[FeI4-] 2 (L = (M e2N)2CS) an d [Fe2I4(C 6H 10(N H -C S -N H M e) 2)2] and a N o te on [F eIL 3]+[F e4S4I3L]~ U lrich Bierbach, W olfgang Saak, D etlev H aase u nd [FeI2L2] (1) and [Fe2I4L3] (2) are obtained from the reaction o f F e l2 and 
  Reference    (Z. Naturforsch. 45b, 45 [1990]; eingegangen am 26 Juli / 18. September 1989) 
  Published    1990 
  Keywords    Thiourea Complexes, Iron C om pounds, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-0045.pdf 
 Identifier    ZNB-1990-45b-0045 
 Volume    45 
127Author    WolfgangA H Errm Ann, JosefK. Felixberger, JosefG. Kuchler, Eberhardt HerdtweckRequires cookie*
 Title    Alkin-Komplexe des Rheniums in hohen Oxidationsstufen Alkyne Complexes of Rhenium in High Oxidation States  
 Abstract    The class o f ^-alkyne complexes o f metals in medium and high oxidation states has been extended by the type C H 3R e 0 2(R C = C R) (3a-i). Exchange o f alkyne for oxo ligands under reducing conditions has been employed as a new general synthesis. C om pounds 3 are thus ob­ tained by reaction o f methyltrioxorhenium(VII) (1) with the alkynes 2 a -i in the presence o f a ca. 1.1-fold molar amount o f polymer-bound triphenylphosphane as reducing agent ( 
  Reference    Z. Naturforsch. 45b, 876—8 (1990); eingegangen am 30. N ovem ber 1989 
  Published    1990 
  Keywords    M ethyloxorhenium Alkynes, Synthesis, Crystal Structures 
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 Identifier    ZNB-1990-45b-0876 
 Volume    45 
128Author    Michael Schäfer, Jürgen Pebler, Beatrice Borgsen, Frank Weller, K. Urt DehnickeRequires cookie*
 Title    21Sb-Mössbauer-spektroskopische und strukturchemische Untersuchungen an Kronenetherkomplexen SbX3(15-Krone-5) mit X = F, Cl, Br, I. Eine Analyse der Orbitalbesetzungszahlen 12lSb-M össbauer-Spectroscopic and Structural Investigations on Crown Ether Complexes SbX3(15-Crown-5) with X = F, Cl, Br, I. A Population Analysis Crown Ether C om plexes SbX3(15-crown-5)  
 Abstract    The crown ether complexes SbX3(15-crown-5) with X = F, Cl, Br, and I have been prepared by reactions o f 15-crown-5 with the corresponding antimony trihalides in acetonitrile solu­ tions. The com pounds were characterized by IR spectroscopy as well as by l21Sb-M össbauer spectroscopy. A m ethod o f orbital population analysis utilizing both M össbauer isomer shifts and quadrupole coupling has been developed for Sb(III) antimony halides and their crown ether com plexes. SbF 3(l 5-crown-5) was also characterized by an X-ray structure determination: Space group P 2 ,/«, Z = 4, 3628 observed unique reflexions, R = 0.032. Lattice dim ensions at 19 °C: a = 891.54(6), b = 1277.26(6), c = 1277.66(7) pm, ß = 95.029(4)3. The com plex has a molecular structure in which the antimony atom is surrounded by three F-atom s with mean bond lengths o f 192.4 pm and by the five oxygen atom s o f the crown ether molecule with mean bond lengths o f 293.9 pm. 
  Reference    Z. Naturforsch. 45b, 1243—1250 (1990); eingegangen am 5. März/9. Mai 1990 
  Published    1990 
  Keywords    Syntheses, IR Spectra, 12lSb-M össbauer Spectra, Crystal Structure 
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 Identifier    ZNB-1990-45b-1243 
 Volume    45 
129Author    Jürgen Silberzahn, Hans Pritzkow, HansPeter LatschaRequires cookie*
 Title    Synthese und Kristallstruktur eines l(A5),4(A5)-Diphosphaazulens sowie dreier 1 -Phospha-1,6a-dihy dropentalene Synthesis and Crystal Structure o f a l(/l5),4(^5)-Diphosphaazulene and of Three 1 -Phospha-1,6a-dihydropentalenes  
 Abstract    The reaction o f acetylene-bis(phosphonous-bisdimethylamide) (1) with tetraphenyl-cyclo-pentadienone (2) yields a 1-phospha-1,6a-dihydropentalene (4), which can be sulfurized with CS2 to give the 1-thio-compound 5, and oxidized with H 20 2 to give the 1-oxo-compound 6. With dim ethyl-acetylenedicarboxylate (7) an amazingly stable l (/ 5),4(A5)-diphosphapen-talene (8) is generated, which reacts further with 7 to yield a l(/.5),4 (/5)-diphosphaazulene (9). The preparation o f the new molecules 4, 5, 6, 9 and the crystal structures o f 5 and 9 are reported. 
  Reference    Z. Naturforsch. 46b, 197—201 (1991); eingegangen am 15. Juni 1990 
  Published    1991 
  Keywords    Phosphororganic Azulene and Dihydropentalenes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0197.pdf 
 Identifier    ZNB-1991-46b-0197 
 Volume    46 
130Author    Frank Weller, Irene Pauls, K. Urt Dehnicke, Gerd BeckerRequires cookie*
 Title    Die  
 Abstract    Reaktionen von Wolframhexachlorid mit überschüssigem 2,2-Dimethylpropylidinphosphan; die Kristallstrukturen von WC15P2(C5H9)3, WC14P5(C5H 9)s und |C3(C4H9)3| +|WC1S(C4H9C -C C 4H9)|-The Reactions of Tungsten Hexachloride with Excess 2,2-Dimethylpropylidynephosphane; the Crystal Structures of WC15P2(C5H9)3, WC14P5(C5H 9)5, and [C3(C4H9)3]+[WC15(C4H9C = C C 4H 9)]- The reaction of tungsten hexachloride with excess 2,2-dimethylpropylidynephosphane, C4H9-C = P , leads to the tungsten phosphaalkyne clusters WC15P2(C5H9)3 and WC14P5(C5H9)5, as well as to the tris(/'-butyl)cyclopropenium pentachloro tungsten alkyne complex [C3(C4H9)3]+[WC15(C4H9C=CC4H9)]-. All complexes were characterized by X-ray structure determinations. WC15P2(C5H9)3: Space group P 2,/«, Z = 8, 4653 observed unique reflexions, R = 0.033. Lat­ tice dimensions at 20 C: a = 1577.8(2), b = 1661.3(1), c = 1869.8(2) pm, ß = 110.64(1)°. The compound has a molecular structure, in which the tungsten atom is surrounded by three chlo­ rine atoms, three carbon atoms with W -C distances of 182, 230, and 231 pm. and by one phosphorus atom with W -P = 246 pm. WC14P5(C5H9)5: Space group P2,/c, Z = 4, 3517 observed unique reflexions, R = 0.043. Lat­ tice dimensions at 20 °C: a = 1770.0(2), b = 1032.9(2), c = 1876.0(3) pm, ß = 102.86(1)°. The complex has a molecular structure, in which the tungsten atom is surrounded by two chlorine atoms, two carbon atoms with W -C distances of 189 and 215 pm, as well as by four phospho­ rus atoms with W -P distances of 242, 250, 264, and 268 pm. [C3(C4H9)3]*[WC15(C4H9C=CC4H9)] : Space group P2l/c', Z = 4, 3284 observed unique re­ flexions, R = 0.052. Lattice dimensions at 20 °C: a = 941.5(3), b = 1762.2(6), c = 1903.5(7) pm, ß = 92.27(3)°. The compound consists of tris(/-butyl)cyclopropenium ions, and anions [WC15(C4H9C=CC4H9)]_, in which the bis(r-butyl)alkyne ligand is coordinated side-on, corre­ sponding to a cyclopropene type structure with W -C distances of 198 pm. 
  Reference    Z. Naturforsch. 46b, 519—529 (1991); eingegangen am 8. November 1990 
  Published    1991 
  Keywords    Phosphaalkyne Clusters of Tungsten, Syntheses, Crystal Structure 
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 Identifier    ZNB-1991-46b-0519 
 Volume    46 
131Author    Rüdiger Staffel, Ulrich Müller, Andreas Ahle, K. Urt DehnickeRequires cookie*
 Title    Die Kristallstruktur von [Na(12-Krone-4)2+l2Se82 * (Se6, Se7) The Crystal Structure o f [Na(12-Crown-4)2+]2Se82 -(Se6, Se7)  
 Abstract    The title com pound was prepared from sodium polyselenide and 12-crown-4 in D M F solution in the presence o f cerium(IlI)chloride in the form o f black needles. The crystal structure determination by X-ray diffraction shows a partially disordered structure, in which the anionic units Se82-■ Se7 and Se82- • Se6 are present in the ratio 0.72/0.28. These units are as­ sociated to layers parallel to (1 0 0); the layers alternate with pseudohexagonal layers o f [N a(12-crown-4)2]+ ions. Space group P i, Z = 2, 3903 observed unique reflections, R = 0.114, w R = 0.084. Lattice dim ensions at -6 5 °C: a = 1247.9(3), b = 1367.8(8), c = 1660(1) pm, a = 94.65(5), ß = 98.94(3), y = 91.10(3)°. 
  Reference    Z. Naturforsch. 46b, 1287—1292 (1991); eingegangen am 8. April 1991 
  Published    1991 
  Keywords    Octaselenide, Cycloheptaselenium, Cyclohexaselenium, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1287 
 Volume    46 
132Author    Dieter Sellmann+, W. Olfgang Kern, Adelgunde Holzmeier, Georg Pöhlmann, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, LXVI  
 Abstract    Substitutions-und Additionsreaktionen an Molybdän-und Wolfram-Schwefel-Zentren von |M (Cl)(NO)('S4)], M = Mo, W, mit Thiolaten SR" (R = Me, 'Pr, w Bu, Ph) und PM e3 ('S4'2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)) Transition M etal Complexes with Sulfur Ligands, LXVI* Substitution and A ddition Reactions at M olybdenum and Tungsten Sulfur Centres of [M(Cl)(NO)('S4')], M = M o, W, with Thiolates SR " (R = Me, 'Pr, "Bu, Ph) and PM e3('S4'2~ = l,2-Bis(2-mercaptophenylthio)ethane(2-)) Since substrate addition and elim ination reactions are essential reactions o f metal sulfur centres in oxidoreductases, we investigated the substitution o f chloride in [Mo(C1)(NO)('S4')](1) ('S4'2-= l,2-Bis(2-m ercaptophenylthio)ethane(2-)) [4] and in the anal­ ogous tungsten complex [W (Cl)(NO)('S4')](2). The chloride ligands in 1 and 2 can easily be substituted by thiolates to give [M (SR)(NO)('S4')] (M = M o, R = Me 3a, 'Pr 3b, "Bu 3c, Ph 3d; M = W, R = Me 4 a , Ph 4b). For these substitution reactions an associative mechanism is suggested. The SR~ ligands act probably as o-n four electron donor ligands to give metal centres with an 18 electron configuration as also found in the amido complexes [M o(N R 2)(NO)('S4')] [4]. 1 and 2 react with PM e3 to yield the adducts [M(PMe3)(Cl)(NO)('S4')] (M = Mo 5, W 6), w hose N M R spectra indicate the formation o f two stereoisomers in a ratio o f about 2:3. 
  Reference    Z. Naturforsch. 46b, 1349—1356 (1991); eingegangen am 28. Januar 1991 
  Published    1991 
  Keywords    Sulfur Complexes, Synthesis, Reactions, Stereochemistry, M olybdenum, Tungsten 
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 Identifier    ZNB-1991-46b-1349 
 Volume    46 
133Author    Yüniu Bai, M. Athias Noltemeyer, H. Erbert, W. RoeskyRequires cookie*
 Title    Synthese und Strukturen von Monoalkylamiden und -imiden des Titans Synthesis and Structures o f M onoalkylam ides and -imides of Titanium  
 Abstract    A new method for the preparation o f m onoalkylam ides o f com position Cp'TiCl2N H R is reported. M e3SnN H R (R = /Bu l a , CH/Pr-, lb) reacts with Cp'TiCl3 with elimination o f M e3SnCl to yield Cp'TiCLNHR (2) (2a: Cp' = C 5H 5, R = /Bu, 2b: Cp' = M e3SiC5H 4, R = t Bu, 2c: Cp' = (M e3Si)?C 5H 3, R = /Bu, 2d: Cp' = M e4C5H, R = /Bu, 2e: Cp' = M e5C5, R = t Bu, 2f: Cp' = C5H 5, R = CH/Pr2, 2g: Cp' = M e3SiC5H 4, R = CH/Pr2, 2h: Cp' = (M e3Si)2C5H3, R = CH/Pr2, 2i: Cp' = M e4C5H , R = CH/Pr2, 2j: Cp' = M e5C5, R = CH/Pr2). Compounds 2 a -2 j are stable and eliminate HC1 only in the presence o f a strong base to form (C5H 5T iC lN /B u)2 (3a) or (M e3SiC5H4T iC lN /B u)2 (3b) from 2 a and 2b, respectively. In 3a the chlorine atom s are substituted by N H /B u groups in boiling T H F by means o f L iN H /Bu to give (C5H 5T iN H /B uN /B u)2 (4). The reactions o f 2 e and 2b with L iN (SiM e3)2-Et20 in the presence o f pyridine yield M e5C5T iC lN /B u • Py (5 a) (Py = pyridine) and M e3SiC5H4T iC lN /B u P y (5 b), respectively. Com pounds 2 e and 5 a have been characterized by X-ray crystal structural analysis. 
  Reference    Z. Naturforsch. 46b, 1357 (1991); eingegangen am 22. März 1991 
  Published    1991 
  Keywords    X -Ray, Synthesis, Titanium, Amides, Imides 
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 Identifier    ZNB-1991-46b-1357 
 Volume    46 
134Author    Stefan Vogler, W. Erner Massa, Kurt DehnickeRequires cookie*
 Title    Über die Reaktion von Wolframhexachlorid mit Se4N 2; Kristallstruktur von PPh4|W Cl5(NSeCl)| On the Reaction of Tungsten Hexachloride with Se4N 2; Crystal Structure of PPh4[WCl5(NSeCl)]  
 Abstract    The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)]. which was characterized by an X-ray structure determination. Space group P 2j, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimen­ sions at -8 0 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; ß = 111.93(3) . The [WC15(NScC1)] ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm. 
  Reference    Z. Naturforsch. 46b, 1625—1628 (1991); eingegangen am 29. Mai 1991 
  Published    1991 
  Keywords    Chloroselenonitrene Complexes of Tungsten, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1625 
 Volume    46 
135Author    Ulrich Bierbach, Wolfgang Saak, Detlev Haase, Siegfried PohlRequires cookie*
 Title    Neutrale und kationische Eisen-Schwefel-Komplexe und -Cluster  
 Abstract    Synthese und Kristallstrukturen von [Fe(SR)2L2l * PhMe und [Fe4S4(SR)2 L2| sowie zur Bildung von [Fe(SR)L3]+, [FeL4]2+, [Fe4S4(SR)L3| + und [Fe4S4L4|2+ (R = 2,4,6-/-Pr3C6H 2; L = SC (N M e2)2) Neutral and Cationic Iron-Sulfur Complexes and Clusters Syntheses and Crystal Structures of [Fe(SR)2 L2] • PhM e and [Fe4S4(SR)2 L2], and on the Form ation of [Fe(SR)L3]+, [FeL4]2+. [Fe4S4(SR)L3]+ and [Fe4S4 L4]2+ (R = 2,4,6-/-Pr3C6H 2; L = SC(NM e2)2) The reaction of [FeLL,] (1; L = SC(NMe,),) with KSR (R = 2,4,6-/-Pr3C6H-,) yields [Fe(SR)2L2] • PhMe (2). 
  Reference    Z. Naturforsch. 46b, 1629—1634 (1991); eingegangen am 13. Juni 1991 
  Published    1991 
  Keywords    Iron Sulfur Complexes and Clusters, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1629 
 Volume    46 
136Author    A. Dalbert Lossin, Gerd Meyer, R. Obert Fuchs, Joachim SträhleRequires cookie*
 Title    [Sm(CH3C 0 0 )3 (H 20)2] * CH 3COOH, ein Essigsäureaddukt des Samarium(III)-acetatdihydrates [Sm(CH3C0 0 )3(H 20 )2] * CH 3COOH, an Acetic Acid Adduct o f Sam arium (III) Acetate Dihydrate  
 Abstract    The crystal structure o f the acetic acid adduct o f the so far unknown samarium(III) acetate dihydrate was determined from single-crystal four-circle diffractometer data. It has the com ­ position [Sm (CH 3C 0 0)3 (H 20) 2] C H 3C 0 0 H containing {[Sm (CH3C 0 0)3 (H 20) 2]}2 dimers and crystallizes in the trigonal system, R 3, a = 2695.1(3), c = 1030.8(4) pm, Vm = 216.97(5) cm 3/m ol, R = 0.041, Rw = 0.030. 
  Reference    Z. Naturforsch. 47b, 179—182 (1992); eingegangen am 5. September 1991 
  Published    1992 
  Keywords    Samarium Acetate, Acetic Acid Adduct, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0179.pdf 
 Identifier    ZNB-1992-47b-0179 
 Volume    47 
137Author    Volker Müller, Gerlinde Frenzen, K. Urt Dehnicke, Dieter FenskeRequires cookie*
 Title    Synthese, FIR-Spektren und Kristallstrukturen der Pentaselenide K2Se5 und [Na(15-Krone-5)l2Se5 Syntheses, F IR Spectra, and Crystal Structures of the Pentaselenides K 2Se5 and [Na( 15-crown-5)]2Se5  
 Abstract    K2Se5 has been prepared by crystallization from a potassium polyselenide solution in D M F. In a similar way [Na(15-crown-5)]2Se5 can be prepared by crystallization from a sodium p oly­ selenide solution in D M F in the presence o f 15-crown-5. Both com pounds were characterized by FIR spectroscopy as well as by X-ray structure determinations. K2Se5: Space group P 2,2,2,, Z -4, 1659 observed independent reflections, R = 0.061. Lat­ tice dim ensions at -9 0 °C; a = 671.5(5), b = 694.9(5), c = 1776.4(9) pm. The com pound crys­ tallizes with the K2S5 type structure. [Na(15-crown-5)]2Se5: Space group P 1, Z = 2, 3026 observed indenpendent reflections, R = 0.140. Lattice dim ensions at -1 0 0 °C: a = 853.7(5), b = 1042.8(10), c = 2011.0(10) pm; a = 88.95(5)°, ß = 79.42(5)°, y = 66.15(5)°. The compound forms an ion triple, in which the sodium ions are coordinated by the five oxygen atoms o f the crown ether molecules as well as by the terminal selenium atom s o f the pentaselenide chain. The rather high R value is a result o f the disordered crown ether molecules. 
  Reference    Z. Naturforsch. 47b, 205 (1992); eingegangen am 23. August 1991 
  Published    1992 
  Keywords    Pentaselenides, Syntheses, FIR Spectra, Crystal Structure 
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 Identifier    ZNB-1992-47b-0205 
 Volume    47 
138Author    Stefan Vogler, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur des Dichloroselenonitren-Komplexes (PPh4)2[WCl5(N SeC l2)| Synthesis and Crystal Structure of the Dichloro-selenonitrene Complex (PPh4)2[WCl5(NSeCl2)]  
 Abstract    The title com pound has been prepared by the reaction o f [WCl4(N SeCl)]2 with PPh4Cl in CH2C12 solution. It forms red crystals, which were characterized by an X-ray structure deter­ 
  Reference    Z. Naturforsch. 47b, 301 (1992); eingegangen am 27. September 1991 
  Published    1992 
  Keywords    Dichloro-selenonitren Complex o f Tungsten, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0301.pdf 
 Identifier    ZNB-1992-47b-0301 
 Volume    47 
139Author    Irina Sens, AlfredDirk Bacher, Ulrich MüllerRequires cookie*
 Title    Natrium-tetraethylammonium-tetrasulfid, N a+NEt4+S42 Synthese und Kristallstruktur Synthesis and Crystal Structure  
 Abstract    N aN E t4S4 was obtained from an equimolar solution of N a2S4 and N E t4Cl in ethanol. Its crystal structure was determined by X-ray diffraction with 4175 observed unique reflexions, R = 0.044. Crystal data: a = 713.4(4), b = 1744.5(9), c = 1204.0(5) pm, ß = 105.8(3)°, space group P 2 ,/«, Z = 4. In the structure, chains consisting of N a + and S42~ ions run in the a direc­ tion, every N a+ being coordinated by four terminal S atom s of S42~ ions (two terminal, one chelating). The chains are separated by the N E t4+ ions. 
  Reference    Z. Naturforsch. 47b, 819—822 (1992); eingegangen am 16. Januar 1992 
  Published    1992 
  Keywords    Sodium Tetraethylammonium Tetrasulfide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0819.pdf 
 Identifier    ZNB-1992-47b-0819 
 Volume    47 
140Author    Henry StrasdeitRequires cookie*
 Title    Synthesis, Spectroscopic and X-Ray Structural Characterization of |Cd(linpen)l2+, a Model for M etal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)  
 Abstract    The isolation of 3,6,9,12-tetraazatetradecane-l,14-diam ine (linear isomer o f pentaethylene­ hexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand tow ards cadmium(II). The solid compounds [Cd(linpen)](BPh4)2 (1), [Cd(linpen)](BPh4)2-2D M SO (2) and [Cd(linpen)](BF4)2 (3) have been isolated and character­ ized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113Cd N M R reso­ nance of 1 is at 351 ppm (0.30 M in DM SO -d6, standard: 0.10 M Cd(C104)2 in D 20). 2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C2/c; a = 19.337(1) A, b = 17.937(1)Ä, c = 18.584(1)Ä, ß = 1 1 1.54(1)°; Z = 4, R = 0.034, Rw = 0.033. 3: P2,/h; a = 8.607(1)Ä, b = 14.851(2)Ä, c = 15.703(2)Ä, ß = 91.21(2)°; Z = 4, R = 0.083, R" = 0.072. Both com pounds contain discrete [Cd(linpen)]2+ complexes. The hexamine wraps ar­ ound the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean C d -N bond lengths are 2.38Ä and 2.37Ä for 2 and 3, respectively. Models for M N 6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)]2+. F or example, loops at the M N 6 site in molecules of linear PEI are proposed. 
  Reference    Z. Naturforsch. 47b, 829—836 (1992); received December 12 1991 
  Published    1992 
  Keywords    Pentaethylenehexamine, Cadmium Complex, Synthesis, Crystal Structure, Polyethyleneimine 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0829.pdf 
 Identifier    ZNB-1992-47b-0829 
 Volume    47 
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