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1991[X]
1Author    SylviaM. Agull, Bernhard Neumüller, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der Polyselenido-Mercurate (PPh4)2|H g(Se4)2| und |Cs(18-Krone-6)|2|H g2(Se4)3l Syntheses and Crystal Structures of the Polyselenido M ercurates (PPh4)2[Hg(Se4)2] and [Cs(18-Crown-6)]2[Hg2(Se4)3]  
 Abstract    (PPh4)2[Hg(Se4)J has been prepared by the reaction o f (PPh4)2[Sn(Se4)3] with H g(C H 3COO)2 in dimethylformamide (D M F) solution. [Cs(18-crown-6)]2[Hg2(Se4)3] has been prepared by the reaction o f a lithium polyselenide solution in D M F with H g(C H 3COO)2 in the presence o f CsBr and 18-crown-6. Both com pounds are obtained as dark red crystals and characterized by X-ray structure determinations. (PPh4) 2[H g(Se4) 2]: Space group P 2,/c, Z = 4, 3021 observed unique reflexions, R = 0.082. Lattice dim ensions at 20 °C: a = 1046.0(3), b = 2129.4(2), c = 2213.1(3) pm,/? = 97.62(2)°. The com pound consists o f PPh4+ ions and anions [Hg(Se4)2]2", in which the mercury atom is a spi-rocenter o f puckered HgSe4 rings. [ Cs(18-crown-6) J2[H g2(Se4)3J: Space group la, Z = 4, 2859 observed unique reflexions, R = 0.074. Lattice dimensions at 20 °C: a = 2018(1), b = 1097.0(2), c = 2317.1(5) pm, ß = 99.40(3)°. The compound forms an ion triple which originates from Cs-Se contacts o f 382 to 390 pm with the [Hg2(Se4)3]2~ ion. The latter can be described as a [FlgtSe^JJ2-ion, which has contacts with a HgSe4 fragment. 
  Reference    Z. Naturforsch. 46b, 985—9 (1991); eingegangen am 12. Dezember 1990 
  Published    1991 
  Keywords    Polyselenido Mercurates, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0985.pdf 
 Identifier    ZNB-1991-46b-0985 
 Volume    46 
2Author    Bernhard NeumüllerRequires cookie*
 Title    Darstellung und Kristallstruktur von [(Me3Si)2CH(7-Pr)InCll2 Synthesis and Crystal Structure o f [(Me3Si)2CH(/-Pr)InCl]2  
 Abstract    The title com pound 1 has been prepared by the reaction o f z-PrlnCl, with LiC H (SiM e3)2 in diethylether at -3 0 °C. The colorless substance 1 was characterized by N M R , IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P 2 ,/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and ß = 101.18(2)°. The unit cell contains two centrosymmetri-cal dimeric molecules. 
  Reference    Z. Naturforsch. 46b, 1539—1543 (1991); eingegangen am 12. April 1991 
  Published    1991 
  Keywords    Diorganoindiumchloride, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1539.pdf 
 Identifier    ZNB-1991-46b-1539 
 Volume    46 
3Author    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 
4Author    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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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0519.pdf 
 Identifier    ZNB-1991-46b-0519 
 Volume    46 
5Author    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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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1287.pdf 
 Identifier    ZNB-1991-46b-1287 
 Volume    46 
6Author    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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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1349.pdf 
 Identifier    ZNB-1991-46b-1349 
 Volume    46 
7Author    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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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1357.pdf 
 Identifier    ZNB-1991-46b-1357 
 Volume    46 
8Author    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 
9Author    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 
10Author    Eberhard Bessler, BrowdoM. Arins Barbosa, Wolfgang Hiller, Johann WeidleinRequires cookie*
 Title    Synthese und Eigenschaften von Tetrakis(trimethylsilylisocyanid)nickel(0), N i(C = N -S iM e 3)4 Synthesis and Properties of Tetrakis(trimethylsilylisocyanide)nickel(0), N i(C = N -S iM e 3)4  
 Abstract    Ni(CNSiMe3)4 (Me = CH,), the first homoleptic isocyanosilane complex, has been prepared by reaction of bis(1,5-cyclooctadiene)nickel(0) with trimethylcyanosilane in ether and charac­ terized by its infrared, Raman spectra, ,3C NMR spectra. 
  Reference    Z. Naturforsch. 46b, 490—494 (1991); eingegangen am 8. November 1990 
  Published    1991 
  Keywords    Tetrakis(trimethylsilylisocyanide)nickcl(0), Synthesis, Vibrational Spectra, 13C NMR Spectra 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0490.pdf 
 Identifier    ZNB-1991-46b-0490 
 Volume    46 
11Author    Dieter Fenske, Sylvia Magull, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von |Rb(18-Krone-6)|2IZn(Se4)(Se6)l Synthesis and Crystal Structure o f [Rb(18-Crown-6)]2[Zn(Se4)(Se6)]  
 Abstract    [Rb(18-crown-6)]-,[Zn(Se4)(Se6)] has been prepared by the reaction o f a lithium polyselenide solution in D M F with zinc acetate in the presence o f rubidium iodide and 18-crown-6. It forms dark red crystals, which were characterized by FIR spectroscopy as well as by an X-ray struc­ ture determination. Space group C 2/c, Z = 4, 3012 observed unique reflections, R = 0.073. Lattice dim ensions at —50 °C: a = 1963.1(14), b = 1125.9(9), c = 2060.3(16) pm,/? = 90.05(3) . The com pound has a com plex ionic structure, in which the zinc atom o f the anion [Zn(Se4)(Se6)]2" is coordinated tetrahedrally by four selenium atoms o f a Se42~ and a Se62~ unit in five and seven membered rings, respectively. The complex cations [Rb(18-crown-6)]+ have Rb • ■ • Se contacts o f 360.7 and 372.0 pm with selenium atoms o f the ZnSe4-ring. 
  Reference    Z. Naturforsch. 46b, 1011—1014 (1991); eingegangen am 6. Februar 1991 
  Published    1991 
  Keywords    Polyselenide Complex o f Zinc, Synthesis, IR Spectrum, Crystal Structure 
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 Identifier    ZNB-1991-46b-1011 
 Volume    46 
12Author    J. Skowronek, W. Preetz, S. M. JessenRequires cookie*
 Title    Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der Acetatochloroditechnetate(III)  
 Abstract    , cis-T ^ C ^ C C F ^ C ^ I^ (L = axiale Donorbase) sowie Kristallstruktur von a s-T c2(0 2CCH3)2Cl4((CH3)2NC0CH3)2 Preparation, Vibrational Spectra and Norm al C oordinate Analysis o f Acetatochloroditechnetates(III), c« -T c2(0 2C CH 3)2C14L2 (L = Axial Donorbase) and the Crystal Structure of ds-Tc2(0 2C CH 3)2Cl4((CFI3)2N C 0C FI3)2 Tc2(0 2C C H 3),C l4(H 20)2 has been prepared by reaction o f [Tc2C18]2" with acetic anhydride and fluoroboric acid. By treatment with the donor bases L = N ,N-dim ethylform am ide (D M F), N ,N-dim ethylacetam ide (D M A A), dimethylsulfoxide (D M SO), triphenylphosphin-oxide (TPO) and pyridine (Py), the green adducts Tc2(0 2CCH3)2Cl4L2 are formed. The structure o f T c,(O .C C H 3),C l4(D M A A), was determined by X-ray diffraction; space group C 2/c with a = 29.604(4), b = 10.895(2), c = 14.404(2) Ä, ß = 97.87(2)°, Z = 8, /?w = 2.7% . The T c -T c distance is 2.1835(7) Ä , the bridging acetate groups are in c/s-positions. The IR and Raman spectra have been recorded at 80 K and assigned according to point group C-,v, supported by a normal coordinate analysis o f Tc2(0 2C C H 3)2C14(D M A A)2 based on a general valence force field. The stretching interaction constant fd(TcTc) is determined to 3.38 m dyn/Ä. With in­ creasing donor strength o f the axial ligands, the intense Raman vibration v(TcTc), showing up to three overtones, is lowered from 311 to 282 cm *1. The <5-<5* transitions o f all adducts are observed at 6 4 8 -6 5 2 nm. 
  Reference    Z. Naturforsch. 46b, 1305—1314 (1991); eingegangen am 4. März 1991 
  Published    1991 
  Keywords    Diacetatotetrachloroditechnetate(III) Adducts, Synthesis, Crystal Structure, Vibrational Spectra, Normal Coordinate Analysis 
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 Identifier    ZNB-1991-46b-1305 
 Volume    46 
13Author    N. Orbert, K. Uhna, Michael Schulten3, Roland Boeseb, Dieter BläserbRequires cookie*
 Title    Synthese und Struktur von l,3?6,8-Tetra-terf-butylcarbazol  
 Abstract    The synthesis o f 1,3,6,8-tetra-/er/-butylcarbazole (2) by the reaction o f carbazole with tert-butyl chloride in the presence o f aluminium chloride is reported. The X-ray structures o f 2 and its diethyl ether adduct are compared. The gap formed by the ter/-butyl groups in 1,8-position has been calculated and compared with that o f the supermesithyl substituent. 
  Reference    Z. Naturforsch. 46b, 1503—1508 (1991); eingegangen am 4. April 1991 
  Published    1991 
  Keywords    l, 3, 6, 8-Tetra-?m -butylcarbazole, Synthesis, X-Ray 
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 Identifier    ZNB-1991-46b-1503 
 Volume    46 
14Author    Fluoro, Petra Neumann, K. Urt Dehnicke, Dieter Fenske, G.Erhard BaumRequires cookie*
 Title    Fluoro-, Chloro-und Bromo-Wolfram(VI)-Alkinkomplexe. Die Kristallstrukturen von [K(18-Krone-6)l[WF5( P h -C = C -H ) | * CH3CN und | WCl4( P h -C = C -S e -/ i -C 4H 9)(C H 3CN)|  
 Abstract    -, Chloro-, and Bromo-Tungsten(VI) Alkyne Complexes. The Crystal Structures of [K(18-Crown-6)][WF5(P h ~ C = C -H)] • C H 3CN and [WCl4(P h -C = C -S e -w -C 4 H9)(CH 3CN)] Several tungsten alkyne complexes o f the type [WC14(R -C = C -H) ] 2 and [WC14(R -C = C -R') ] 2 have been prepared by reactions o f WC16 with the alkynes in the presence o f C2C14. Treat­ ing with BrSiMe3 leads to corresponding bromo com plexes, whereas reactions o f N aF and KF, respectively, in acetonitrile solution in the presence o f crown ethers yield the fluoro complexes [N a(l 5-crown-5)][WFs(R -C = C -R ') ] and [K(18-crown-6)][W F5(R -C = C -R ') ] , respectively. All complexes were characterized by IR and l3C N M R spectroscopy. The crystal structures o f [K(18-crown-6)][W F5(P h -C = C -H) ] C H 3CN and [WCl4(P h -C = C -S e -« -C 4 H9)(C H 3C N)] have been determined by X-ray methods. [K(18-crown-6)][W F5(P h -C = C -H ] C H 3 CN: Space group P 2,, Z = 2, 8555 observed unique reflections, R = 0.034. Lattice dim ensions at -7 0 °C: a = 1199.4(3), b = 893.4(2), c = 1351.8(3) pm, ß = 109.73(3)°. The com pound forms ion pairs via three K -F contacts with bond lengths o f 262.0, 282.7, and 293.3 pm; the potassium ion is thus nine-fold coordinated by the six oxygen atoms o f the crown ether molecule and by three fluoride ligands. The alkyne ligand is bonded side on to the tungsten atom o f the [W F5(P h -C = C —H)] unit with WC bond lengths o f 202.4 and 202.6 pm, respectively. [WCl4(P h -C = C -S e -t t -C 4 H9)(C H 3C N)]: Space group P 2 Ja, Z = 4, 4595 observed unique reflections, R = 0.058. Lattice dim ensions at -7 0 °C: a = 1030.3(5), b = 1596.3(9), c = 1170.9(7) pm, ß = 104.28(3)°. The com pound has a molecular structure, in which the tungsten atom is seven-fold coordinated by four chloride ligands, by the two alkyne carbon atom s (WC bond lengths 200 and 203 pm), and in trans position to the latter by the nitrogen atom o f the acetonitrile molecule with a W -N bond length o f 226 pm. 
  Reference    Z. Naturforsch. 46b, 999—1010 (1991); eingegangen am 4. Februar 1991 
  Published    1991 
  Keywords    Tungsten Alkyne Complexes, Synthesis, IR Spectra, 13C N M R Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0999.pdf 
 Identifier    ZNB-1991-46b-0999 
 Volume    46 
15Author    EnriqueG. Utiérrez-PueblaRequires cookie*
 Title      
  Reference    Z. Naturforsch. 46b, 1113 (1991); eingegangen am 9. Januar 1991 
  Published    1991 
  Keywords    Hexachlorodicuprates, Tetrachlorocuprates, 3-D iethylam ino-5-phenyl-1, 2, 4-dithiazolium Salts, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1113_n.pdf 
 Identifier    ZNB-1991-46b-1113_n 
 Volume    46 
16Author    Alfred Zinn, Henning Von Arnim, Werner Massa, Michael Schäfer, Jürgen Pebler, K. Urt DehnickeRequires cookie*
 Title    [P h -C (  
 Abstract    N S iM e3)2]2FeO ; ein Amidinatokomplex von Eisen(III) mit verzerrt trigonal-bipyramidaler Struktur [P h -C (N S iM e3)2]2FeCl; an Amidinato Complex o flro n (III) with a Distorted Trigonal-Bipyramidal Structure The am idinato complex [P h -C (N S iM e3)2]2FeCl has been prepared by the reaction o f FeOCl with the amidine P h -C (N S iM e3)[N(SiM e3)2] in acetonitrile/THF in the form o f dark red m ois­ ture sensitive single crystals. The complex was characterized by IR spectroscopy, by its 57Fe-M össbauer spectra, as well as by an X-ray structure determination. Space group P i, Z = 2, 3180 observed unique reflections, R = 0.068. Lattice dimensions at -8 0 C: a = 1210.4(2), b = 1272.7(3), c = 1316.0(3) pm; a = 67.81(3)°, ß = 76.14(3)°, y = 67.19(3)°. The com plex has a molecular structure in which the iron atom is surrounded in a distorted trigonal-bipyramidal fashion with the chlorine ligand and two nitrogen atoms o f different amidinato chelates in equatorial positions. The remaining nitrogen atom s occupy the apical positions. 
  Reference    Z. Naturforsch. 46b, 1300 (1991); eingegangen am 28. Februar 1991 
  Published    1991 
  Keywords    Am idinato Complex o f Iron, Synthesis, IR Spectra, 57Fe M össbauer Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1300.pdf 
 Identifier    ZNB-1991-46b-1300 
 Volume    46