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1988[X]
1Author    W. Preetz, C. SartoriRequires cookie*
 Title    Darstellung und Schwingungsspektren des 13 C-und 18 0-markierten rrans-Dioxotetracyanoosinats(VI), [0s0 2 (CN) 4 ] 2 ~ Preparation and Vibrational Spectra of 13 C and ls O Labelled mms-Dioxotetracyanoosrnate(VI), [0s0 2 (CN) 4 ] 2  
 Abstract    Through careful acidification of the aqueous solution of [0s0 2 (0H) 4 ] 2 ~ in the presence of CN or 13 CN~ with acetic acid, [0s0 2 (CN) 4 ] 2 " or [OsO : (13 CN) 4 ] 2:: are formed, respectively. The reaction of 0s 18 0 4 and tetrabutylammonium cyanide with glacial acetic acid in anhydrous methanol yields [0s 18 0 2 (CN) 4 ] 2 ~. The shifts of the infrared and Raman bands of the isotopically labelled complexes are in good agreement with Teller-Redlich calculations. The degenerate E modes, expected for tetragonal symmetry, are split by approx. 15 cm ', indicating an orthorhombic distortion of the complex ion in the solid state. Therefore, all the observed IR-and Raman frequencies are assigned according to point group D 2h . For the complex containing an 16 0 = 0s= 18 0 axis, the symmetry is lowered to C 2v , and the rule of mutual exclusion is restricted. This results in a weak absorption in the infrared spectrum of the Raman active symmetric OsO stretching vibration and vice versa a weak band in the Raman spectrum for the antisymmetric infrared active mode. 
  Reference    (Z. Naturforsch. 43b, 94—98 [1988]; eingegangen am 11. September 1987) 
  Published    1988 
  Keywords    /rans-Dioxotetracyanoosmate(VI) Isotopic Labeling, IR Spectra, Raman Spectra 
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 Identifier    ZNB-1988-43b-0094 
 Volume    43 
2Author    Eberhard Böhm, Kurt Dehnicke, Johannes Beck, Wolfgang Hiller, Joachim Strähle, Andreas Maurer, Dieter FenskeRequires cookie*
 Title    Die Kristallstrukturen von Ph 3 PNPh, [Ph 3 PN(H)Ph][AuI 2 ] und von 2,3-Bis(triphenylphosphoranimino)maIeinsäure-N-methyIimid The Crystal Structures of Ph 3 PNPh, [Ph 3 PN(H)Ph][AuI 2 ] and of 2,3-Bis(triphenylphosphoranimino)maleic Acid-N-methylimide  
 Abstract    [Ph 3 PN(H)Ph][AuI 2 ] (2) is formed by the reaction of Aul with N-Phenyl-iminotriphenylphos-phorane, Ph 3 PNPh in a toluene suspension. 2,3-Bis(triphenylphosphinimino)maleic acid-N-methylimide (3) has been prepared by the Staudinger reaction of 2,3-bis(azido)maleic acid-N-methylimide with PPh, in THF solution in the form of red crystals. Crystal structure determina-tions of three iminophosphoranes were carried out by X-ray methods. Ph 3 PNPh (1): space group P2]/c, Z = 4, 2176 independent observed reflexions, R = 0.057. Lattice dimensions (-30 °C): a = 1126.4, b = 1148.6, c = 1476.0 pm; ß = 97.21°. The compound forms monomeric molecules with P=N = 160.2 pm and an PNC angle of 130.4°. [Ph 3 PN(H)Ph][AuP] (2): space group PI, Z = 2, 1780 independent observed reflexions, R = 0.057. Lattice dimensions (18 °C); a = 824.9, b = 1022, c = 1476.2 pm; a = 89.23°, ß = 87.41°, y = 85.65°. The compound consists of ions [Ph 3 PN(H)Ph]® with P=N = 162.4 pm and PNC = 129.3°, and anions [Aul 2 ] e with Au-I = 261.9 and 259.3 pm, IAuI = 176.8°. (PhiP) 2 N-,C 4 0 2 (NMe) (3): space group PI, Z = 2, 4972 independent observed reflexions, R = 0.050. Lattice dimensions (-90 °C): a = 904.7, b = 993.8, c = 2017.4 pm; a = 101.55°, ß = 96.39°, y — 105.81°. The compound forms monomeric molecules with ^«-conformation of the two NPPh 3 groups. Bond lengths: P=N = 157.1; 155.3 pm, bond angles: PNC = 133°; 136°. 
  Reference    Z. Naturforsch. 43b, 138—144 (1988); eingegangen am 2. September/6. November 1987 
  Published    1988 
  Keywords    Iminophosphoranes, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-0138 
 Volume    43 
3Author    Cl, Br, Rolf Minkwitz, Arnulf WernerRequires cookie*
 Title    Methyl(trifluormethyl)haIogensulfonium-Salze [ 1 ] Halogen = F, CI, Br, I Methyl(trifluoromethyl)halosulfonium Salts [1]  
 Abstract    The preparation and spectroscopic characterization of the halosulfonium salts CH ,(CF,)SHal + A (Hal = F, Cl, Br, I, A" = AsF 6 ~~, SbF 6 ~, SbCl A ") is reported. The compounds are synthesized by the reaction of the sulfane CH,SCF, with XeF + MF h ~, Cl.F+AsFf,", Cl 2 /AsF 5 , Cl 2 /SbCl 5 , Br : /AsF 5 , or I 3 + MF 6 ~ (M = As, Sb), resp., at low temperatures. 
  Reference    Z. Naturforsch. 43b, 403—411 (1988); eingegangen am 10. Dezember 1987 
  Published    1988 
  Keywords    Preparation Raman Spectra, NMR Spectra, IR Spectra 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0403.pdf 
 Identifier    ZNB-1988-43b-0403 
 Volume    43 
4Author    Fritjof Schmock, Aida El-Kholi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Synthesis and Crystal Structure of PPh 3 Me[HS0 4 ]  
 Abstract    PPh 3 Me[HS0 4 ] was prepared by the reaction of (PPh,Me)I with silver sulfate in aqueous solution. OPPh : Me and benzene being the by-products. The title compound was characterized by its IR spectrum as well as by an X-ray structure determination (1730 observed independent reflexions, R = 0.043). Crys-tal data: a = 910.4(3). b = 1587.8(4), c = 1294.2(6) pm, ß = 105.52(3)°. space group P2,/c t Z = 4. The structure consists of PPh,Me® cations and of HOSO, 0 ions that are associated via strong hydrogen bonds to dimeric centrosymmetric units. 
  Reference    Z. Naturforsch. 43b, 1069—1071 (1988); eingegangen am 13. April 1988 
  Published    1988 
  Keywords    Triphenylmethylphosphonium Hydrogensulfate, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1069_n.pdf 
 Identifier    ZNB-1988-43b-1069_n 
 Volume    43 
5Author    W. Preetz, A. Heinrich, J. ThesingRequires cookie*
 Title    c/oso-Halogenohydrohexaborate, IV Protonierung, Deuterierung und Schwingungsspektren von c/aso-Hexaboraten c/oso-Halogenohydrohexaborate, IV Protonation, Deuteration and Vibrational Spectra of c/oso-Hexaborates  
 Abstract    The weak Brönsted acids B 6 H 7 ~ and XB^H,", X = Cl, Br, I; pk a : 7-4,75, are formed by protonation of B 6 H h 2 ~ and XB 6 H 5 2 respectively. The deuteration rates, evaluated from inte-grated IR band intensities of the BH and BD stretching vibrations, are linearly dependent on the mole fractions of the protonated species, and decrease with increasing degree of halogenation in the series Cl>Br>I. H atoms trans-positioned to halogens are exchanged 100 times more rapidly than the remaining ones. The activation energy for the H/D exchange amounts to 76 ± 1,5 kJ/mol for B 6 H 7 ". The lower symmetry of the protonated borates is evident from additional IR and Raman bands. They are distinguished from the corresponding Brönsted bases by a high frequency shift of the BH stretching vibrations in the order of 100 cm '. Due to the pH dependent equilib-rium B h H (S 2 ~/B (,H 7 " and different solubilities of the tetrabutylammonium salts, the separation of BF,H 6 2 "/B 12 H| 2 2 " mixtures is achievable. In alkaline solutions the very soluble B ft H 6 2 ~ is present, whereas (TBA) 2 B, : HI : precipitates quantitatively. By subsequent cautious acidification of the supernatant, insoluble (TBA)B 6 H 7 is obtained. 
  Reference    Z. Naturforsch. 43b, 1319—1326 (1988); eingegangen am 16. Juni 1988 
  Published    1988 
  Keywords    Halogenohydrohexaborates, Protonation Deuteration, IR Spectra, Raman Spectra 
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 Identifier    ZNB-1988-43b-1319 
 Volume    43 
6Author    A. Heinrich, W. PreetzRequires cookie*
 Title    Darstellung und Schwingungsspektren von Alkyl-und Rhodanohydrohexaboraten Preparation and Vibrational Spectra of Alkyl and Rhodano Hydrohexaborates  
 Abstract    Treatment of B 6 H 6 2 " with iodoalkanes and (SCN) 2 in organic solvents affords the monosubsti-tuted protonated hexaborates RB 6 H 6 ", R = CH 3 , C 2 H 5 < C 3 H 7 , C 4 H 9 , C 8 H 17 and SCN, respective-ly. The acidity constants of these weak Brönsted acids range for the alkylated species from 8.8 to 9.6, and for R = SCN the pk a value is ~5. From basic solutions the salts Cs 2 RB 6 H 5 can be precipitated, which show band patterns in the IR and Raman spectra typical for monosubstituted hydrohexaborates. The protonated compounds RB 6 H 6 " are distinguished from the corresponding Brönsted bases RB 6 H 5 2 " by a high frequency shift of the BH stretching vibrations in the order of 100 cm" 1 . For Cs 2 (SCN)B 6 H 5 , S coordination of SCN" is supposed because of the high frequency of v CN : 2144 cm" 1 . 
  Reference    Z. Naturforsch. 43b, 1327—1331 (1988); eingegangen am 8. Juli 1988 
  Published    1988 
  Keywords    Alkylhydrohexaborates, Rhodanohydrohexaborate, Protonation, IR Spectra, Raman Spectra 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1327.pdf 
 Identifier    ZNB-1988-43b-1327 
 Volume    43 
7Author    Abderraouf Khabou, Kurt Dehnicke, Kurt Findeisen, Farbenfabriken Bayer, Bayer-WerkD. Leverkusen, -5090 Leverkusen, Dieter FenskeRequires cookie*
 Title    Molybdännitridtrichlorid-2,3,3-trichloracrylnitril, [M0NCI3 * NC-C 2 C1 3 ] 2 Synthese, IR-Spektrum und Kristallstruktur Molybdenumnitridetrichloride-2,3,3-trichloroacrylnitrile, [MONC1 3 * NC—C 2 C1 3 ] 2 Synthesis, IR Spectrum, and Crystal Structure  
 Abstract    [MONC1 3 -NC —C 2 C1 3 ] 2 has been prepared by the reaction of MONC1 3 with trichloromethyl isocyanidedichloride, CC1 3 NCC1 2 , in CH 2 C1 2 suspension. The compound forms redbrown. mois-ture sensitive crystals, which were characterized by their IR spectrum as well as by a crystal structure determination (2482 independent observed reflexions, R = 0.048). Crystal data (-70 °C): Space group P2,/c, Z = 2, a = 674.2(2); b = 2128.2(11); c = 786.0(4) pm: ß = 102.81(3)°. [MONC1 3 • NC-C 2 C1 3 ] 2 forms centrosymmetric dimeric molecules via chloro bridges with Mo-Cl bond lengths of 240.7 and 276.0 pm. The longer MoCl bond of the MOC1 2 MO ring is caused by the trans influence of the nitride ligand; the MoN bond length of 167 pm corresponds with a triple bond. The 2,3,3-trichloroacrylnitrile ligand is bonded by its nitrogen atom with a bond length of Mo —N — 216 pm; the Mo-N=C—C sequence is almost linear with a remarkable short C—C bond of 143.0 pm. 
  Reference    Z. Naturforsch. 43b, 1616—1620 (1988); eingegangen am 19. Juli 1988 
  Published    1988 
  Keywords    Molybdenumnitridetrichloride-233-trichloroacrylnitrile, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-1616 
 Volume    43 
8Author    Dieter Fenske, Eberhard Böhm, Kurt Dehnicke, Joachim SträhleRequires cookie*
 Title    N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, (Me 3 SiNPPh 3 * CuCl 2 ]2 Synthese und Kristallstruktur N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me 3 SiNPPh 3 * CuCl : ] 2 Synthesis and Crystal Structure  
 Abstract    The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl 4 /C 2 H 5 OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me 3 SiNPPh 3 • CuCl 2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; ß = 94.27°; space group P2,/« with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu 2 Cl 2 ring (Cu —CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu —CI = 221 pm) and the N atom of the Me,SiNPPh 3 ligand (Cu —N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms. 
  Reference    (Z. Naturforsch. 43b, 1 [1988]; eingegangen am 4. September 1987) 
  Published    1988 
  Keywords    N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-0001 
 Volume    43 
9Author    Manfredo Hörner, Wolfgang Hiller, Joachim Strähle, GeorgeM. SheldrickRequires cookie*
 Title    Synthese, Eigenschaften und Kristallstruktur von (NH 4 )NbOBr 4 Synthesis, Properties and Crystal Structure of (NH 4 )NbOBr 4  
 Abstract    (NH 4)NbOBr 4 is obtained as air sensitive, light red crystals from NH 4 Br and NbBr 5 in a sealed glass ampoule at 420 °C, whereby the oxygen presumably originates from the glass surface. The compound crystallizes in the monoclinic space group C2/m with a — 1269.9(1), b = 1384.7(2). c = 773.0(2) pm, ß = 114.44(2)° and Z = 6. The structure is built up by NH 4 + cations and polymeric NbOBr 4 anions. Symmetrical linear oxo bridges with Nb-O = 199 pm connect square planar NbBr 4 units to form endless chains arranged in planes parallel (010). Neighbouring NbBr 4 units are in eclipsed as well as staggered orientations. The NH 4 + cations are located between the planes of parallel NbOBr 4 " chains. The vibrational frequencies of the IR and Raman spectrum are assigned. 
  Reference    Z. Naturforsch. 43b, 981—984 (1988); eingegangen am 25. März 1988 
  Published    1988 
  Keywords    Ammonium Tetrabromooxoniobate(V), Synthesis, Crystal Structure, Raman Spectra, IR Spectra 
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 Identifier    ZNB-1988-43b-0981 
 Volume    43 
10Author    ;.M = Ti, ZrDieter Fenske, Eva Hartmann, Kurt DehnickeRequires cookie*
 Title    N,N'-Bis(trimethylsilyl)benzamidinato-Koniplexe von Titan und Zirkon. Die Kristallstrukturen von [C 6 H 5 -C(NSiMe3) 2 MCl 3 ] 2 ; M = Ti, Zr N,N'-Bis(trimethylsilyl)benzamidinato Complexes of Titanium and Zirconium. The Crystal Structures of [C 6 H 5 -C(NSiMe 3 ) 2 MCl 3 ]  
 Abstract    The N,N'-bis(trimethylsilyl)benzamidinato complexes [C 6 H 5 -C(NSiMe 3) 2 MCl 3 ] 2 (M = Ti. Zr) have been prepared by the reactions of N,N,N'-tris(trimethylsilyl)benzamidine, [C 6 H 5 — C(NSiMe 3)N(SiMe 3) 2 ] with titanium tetrachloride, and zirconium tetrachloride, respec-tively. The compounds form moisture sensitive, dark red (Ti) and white (Zr) crystals, which were characterized by crystal structure determinations. [C 6 H 5 —C(NSiMe 3) 2 TiCl 3 ] 2 : space group P2,/rc. Z = 2, 4373 observed independent reflexions, R = 0.034. Lattice dimensions (-90 °C): a — 959.0(8); b = 1196.5(8); c = 1770.9(11) pm; ß = 93.79(4)°. [C 6 H 5 -C(NSiMe 3) 2 ZrCl 3 ] 2 : space group P2,/«. Z = 2, 3160 observed independent reflexions, R = 0.031. Lattice dimensions (-90 °C): a = 971.6(7); b = 1222.2(9); c = 1792.9(10) pm; ß = 93.51(5)°. Both complexes crystallize isotypically, forming centrosymmetric dimeric molecules via chloro bridges with bond lengths of 242.0 and 253.8 pm (Ti), and of 253.7 and 264.9 pm (Zr). The metal atoms complete their distorted octahedral surroundings with two chlorine ligands and the nitrogen atoms of the chelating amidinato ligand. The N atoms of the amidinato group are in equatorial and axial positions. This accounts for the different metal-nitrogen bond lengths of 207 pm (ax) and 199 pm (eq) in the titanium compound and 219 pm (ax) and 214 pm (eq) in the zirconium complex. 
  Reference    Z. Naturforsch. 43b, 1611—1615 (1988); eingegangen am 22. Juni 1988 
  Published    1988 
  Keywords    N, N'-Bis(trimethylsilyl)benzamidinato Complexes, Titanium, Zirconium, Syntheses, IR Spectra 
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 Identifier    ZNB-1988-43b-1611 
 Volume    43 
11Author    Astrid Görge, Kurt Dehnicke, Dieter FenskeRequires cookie*
 Title    N-Chlornitrenokomplexe des Wolframs: WC1 4 (NC1) und [CH 3 CN-WC1 4 (NC1)] N-Chloro-Nitrene Complexes of Tungsten: WC1 4 (NC1) and [CH 3 CN-WC1 4 (NC1)]  
 Abstract    WC1 4 (NC1) has been prepared as a red-brown crystal powder by the reaction of tungsten hexacarbonyl with excess nitrogen trichloride in boiling CC1 4 . The complex is associated via chloro bridges, forming dimeric units, according to the IR spectrum. Thermal decomposition at 200 °C leads to tungsten nitride trichloride, WNC1,. With acetonitrile, WC1 4 (NC1) reacts with formation of the monomeric complex [CH,CN-WC1 4 (NC1)], which was characterized by its IR spectrum as well as by an X-ray structure determination. Crystal data: space group P2,/m, Z = 2 (1387 independent observed reflexions, R — 0.07). Lattice dimensions at 20 °C: a = 590.4(3), b = 729.0(3), c = 1124.6(4) pm, ß = 100.63(2)°. The complex forms monomeric molecules, in which the tungsten atom has a distorted octahedral environment of four chlorine atoms in equatorial positions, and the acetonitrile molecule in fram-position to the W=N —Cl group. Bond lengths WN = 172 and NCI -161 pm; bond angle WNC1 = 175.5°. 
  Reference    Z. Naturforsch. 43b, 677—681 (1988); eingegangen am 26. Januar 1988 
  Published    1988 
  Keywords    Synthesis, IR Spectra, X-Ray, N-Chloro-Nitrene-Tungsten Tetrachloride, Acetonitrile Adduct 
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 Identifier    ZNB-1988-43b-0677 
 Volume    43 
12Author    Karin Völp, Gerhard Baum, Werner Massa, Kurt DehnickeRequires cookie*
 Title    [Na-15-Krone-5][MoF 2 Cl2(N 3 S2)]; Synthese und Kristallstruktur [Na-15-Crown-5][MoF 2 Cl 2 (N 3 S 2 )]; Synthesis and Crystal Structure  
 Abstract    The cyclothiazeno complex [Na-15-crown-5][MoF 2 Cl 2 (N 3 S 2)] has been prepared by the reaction of sodium fluoride with [MOC1 3 (N 3 S 2)] 2 in acetonitrile solution in the presence of [15-crown-5], The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion (3560 observed independent reflexions, R = 0.039). Crystal data: monoclinic, P2,//?, Z = 4; a = 1044.8(2); b = 1513.7(2); c = 1363.8(3) pm; ß = 104.33(2)°. The structure consists of ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule and by the two fluorine ligands of the [MOF 2 C1 2 (N 3 S 2)]~ unit. The molybdenum atom is a member of the planar MON 3 S 2 ring; the fluorine atoms are coordinated in trans position to the nitrogen atoms of the cyclothiazeno ring. 
  Reference    Z. Naturforsch. 43b, 1235—1239 (1988); eingegangen am 7. Juni 1988 
  Published    1988 
  Keywords    Fluoro-Chloro-Cyclothiazeno Complex of Molybdenum(VI), Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-1235 
 Volume    43