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1989[X]
1Author    Ekkehard Lindner, Robert SpeidelRequires cookie*
 Title    Neuartige basische Liganden für die homogenkatalytische Methanolcarbonylierung, XXI [1] Synthese und Eigenschaften von (Ether-Phosphan)-Platin-Komplexen Novel Basic Ligands for the Homogenous Catalytic Methanol Carbonylation, XXI [1] Synthesis and Properties of (Ether-Phosphane) Platinum Complexes  
 Abstract    The (ether-phosphane) complexes m -C l2Pt(Ph: P ~ D)2 (2a, b) [D = C H 2C4H 70 (a). C H 2C4H 70 2 (b)] are obtained by reaction of Ph2P ~ D (la , b) with either K2PtCl4 or Cl2Pt(CO D) (C O D = 1,5-cyclooctadiene). Both Cl ^anions are abstracted from 2a, b using A gSbF(1 to give the cationic bischelate complexes [Pt(Ph2P D)2][SbFh]2 (5a, b). The stepwise cleavage and reform a­ tion of Pt —O bonds in (ether-phosphane) platinum complexes is dem onstrated bv the sequence 5a —> [rä -(P h 2P D)(Ph2P ~D)P tC l][S bF 6] (6 a) -* [rra«5-(Ph2P ~ D)2PtC O (C l)][SbF6] (7 a) -* 5a, when 5a, 6 a, and 7a are reacted with KC1. CO, and AgSbF,,, respectively. Reduction of 2a with N aB H 4 results in the form ation of rra/2s-H 2Pt(Ph2P ~ D)2 (4a). In the presence of HC1 2a js re­ formed. Excess N aBH 4 or heating of 4a yields the bischelate platinum(O) complex Pt(P h: P D)2 (3a), which is also jso lated by reduction of 2a with sodium amalgam. A general method for obtaining P t(P h2P D)2 (3 a —c) [D = C H 2C H 2O C H , (c)] is the substitution of C O D in P t(C O D)2 by the ether-phosphanes l a —c. The structures and bonding properties of the com pounds 2 —7 are discussed on the basis of their 31P {1H } NMR and IR spectra. 
  Reference    Z. Naturforsch. 44b, 437—443 (1989); eingegangen am 20. D ezem ber 1988 
  Published    1989 
  Keywords    Ether-Phosphanes Platinum Complexes, 3iP {'H} NMR Spectra, IR Spectra 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0437.pdf 
 Identifier    ZNB-1989-44b-0437 
 Volume    44 
2Author    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 
3Author    Jochen Ellermann, Norbert WillRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 104 [1] Gold-, Palladium-und Platinchlorokomplexe von (±)-2-[N,N-Bis(2-diphenylphosphinoethyl)amino]-tetrahydro- 2 //-l,3,2-oxazaphosphorin-2-oxid Chemistry of Polyfunctional Molecules, 104 [1] Gold-, Palladium-and Platinumchlorocomplexes of (±)-2-[N,N-Bis(2-diphenylphosphinoethyl)amino]-tetrahydro- 2 H-l ,3,2-oxazaphosphorine-2-oxide  
 Abstract    Reaction o f AuC1(C8H i4) with (Ph2PC H 2C H 2)2N -P (O)N (H)C H 2C H 2CH 20 (2) gives the 
  Reference    (Z. Naturforsch. 44b, 127 [1989]; eingegangen am 2. N ovem ber 1988) 
  Published    1989 
  Keywords    Noble M etals, IR Spectra, Raman Spectra, NM R Spectra 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0127.pdf 
 Identifier    ZNB-1989-44b-0127 
 Volume    44 
4Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0278.pdf 
 Identifier    ZNB-1989-44b-0278 
 Volume    44 
5Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1003.pdf 
 Identifier    ZNB-1989-44b-1003 
 Volume    44 
6Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1155.pdf 
 Identifier    ZNB-1989-44b-1155 
 Volume    44 
7Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1325_n.pdf 
 Identifier    ZNB-1989-44b-1325_n 
 Volume    44 
8Author    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 
9Author    P. E. Rlhöfer, W. PreetzRequires cookie*
 Title    Darstellung und Schwingungsspektren der 35CI/37Cl-markierten Fluoro-Chloro-Platinate(IV) Preparation and Vibrational Spectra of 35C1/ Cl Labelled Fluoro-Chloro-Platinates(IV)  
 Abstract    A ll com ponents of the two series Cs2[PtF"35Cl6_"] and Cs2[PtF"37ClA_"], including the pairs of geom etric isomers for n = 2 ,3 , 4, have been prepared and isolated by ion exchange chrom atogra­ phy on D E A E cellulose. The highly resolved low temperature (80 K) IR and Raman spectra of the pure isotopom ers show distinctive isotopic shifts for different vibrational m odes up to 10 cm -1 . The excellent agreem ent o f the observed values with Teller-R edlich calculations verifies the assignm ent of all stretching and especially o f the narrow deform ation bands. For trans -com plexes containing C l—P t— Cl axes, the lowered of mutual exclusion. 
  Reference    Z. Naturforsch. 44b, 619 (1989); eingegangen am 8. Februar 1989 
  Published    1989 
  Keywords    Fluoro-C hloro-Platinates(IV ), Isotopom ers, Teller-Redlich Calculation, IR Spectra, Raman Spectra 
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 Identifier    ZNB-1989-44b-0619 
 Volume    44 
10Author    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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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-0889.pdf 
 Identifier    ZNB-1989-44b-0889 
 Volume    44 
11Author    PeterH. Ofacker, Claus Friebel, Kurt Dehnicke, Petra Bäuml, Wolfgang Hiller, Joachim SträhleRequires cookie*
 Title    Über die Reduktion von Alkinkomplexen des Molybdäns und Wolframs in hohen Oxidationsstufen. Die Kristallstruktur von MoCI3(THF)3 On the Reduction of Alkyne Complexes of M olybdenum and Tungsten in High Oxidation States. The Crystal Structure of MoC13(T H F)3  
 Abstract    The reduction of the tungsten alkyne complexes [WC14(R C = C R)]2 (R — Ph. SiMe3) with cobaltocen in T H F solutions leads to the complexes [CoCp2]2[WCl4(R C = C R)]2 (R = Ph (i); R — SiMe3 (2)), as green, oxygen sensitive crystalline powders. Reduction of [WCl4(M e3SiC =C SiM e3)]2 and of[M oC l4(P hC = C P h)]2 with sodium naphthalide in T H F solutions in the presence of 15-crown-5 gives [Na-15-crown-5]3[W2Cl9], and MoC13(T H F)3, respectively. All compounds have been characterized by IR spectroscopy, and 1 and 2, in addition, by their E PR spectra. The crystal structure of MoC13(T H F)3 was determ ined by X-ray m ethods. Space group P2,/c, Z — 4, 2642 observed unique reflexions, R = 0.050. Lattice dim ensions at 20 °C: a = 888.4(2), b = 1281.5(3), c = 1535.2(3) pm, ß = 92.17(2)°. The com pound forms m onom eric octahedral molecules with a meridional arrangem ent of the ligands. 
  Reference    Z. Naturforsch. 44b, 1161 (1989); eingegangen am 28. Juni 1989 
  Published    1989 
  Keywords    Alkyne Complexes of Molybdenum and Tungsten, R eduction, E PR Spectra, Crystal Structure, IR Spectra 
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 TEI-XML for    default:Reihe_B/44/ZNB-1989-44b-1161.pdf 
 Identifier    ZNB-1989-44b-1161 
 Volume    44