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1Author    Birgit Lehnis, Joachim SträhleRequires cookie*
 Title    Synthese und Kristallstruktur von C83(AuBr 4 ) 2 Br3 Synthesis and Crystal Structure of Cs3(AuBr4) 2 Br 3  
 Abstract    Cs3(AuBr4)2Br3 is obtained in the form of red needles by adding the stoichiometric amount of CsBr to a solution of HAuBr4 and Br3~ in aqueous HBr. The salt decomposes slowly at room temperature to form a mixed-valent, cubic bromo aurate(I,III), in which the linear AuBr 2 ~ ions are partially substituted by Br3~ ions. At 140 °C Cs 2 Au 2 Bre and CsBr are formed. Cs3(AuBr4) 2 Br3 crystallizes monoclinic with four formula units in the space group P2i/c. The structure is built up by AuBr 4 ~ and Br3~ anions and Cs+ cations. An average Au-Br distance of 242.2 pm was found for the square planar AuBr 4 ~ ion. The linear Br3~ groups are almost symmetrical with Br-Br distances of 254.0 and 256.2 pm. Therefore only two vibrations are observed in the IR spectrum: Vas = 172, <5 = 56 cm -1 . The absorptions of the AuBr 4 _ groups are: vas = 250, <5as= 113, y — 102 cm -1 . 
  Reference    Z. Naturforsch. 36b, 1504—1508 (1981); eingegangen am 8. September 1981 
  Published    1981 
  Keywords    Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/36/ZNB-1981-36b-1504.pdf 
 Identifier    ZNB-1981-36b-1504 
 Volume    36 
2Author    Hans Zimmer, Madhusudan Jayawant, Adel Amer, BruceS. AultRequires cookie*
 Title    Reactions of Alkylamino-and Dialkylaminotriphenylphosphonium Halides with Halogens and Interhalogen Compounds; Formation of Alkylaminotriphenylphosphonium Polyhalides  
 Abstract    Alkylamino-and cycloalkylaminotriphenylphosphonium halides react with elemental halogens or interhalogen compounds to afford alkylamino-or cycloalkylaminotriphenyl-phosphonium trihalides. The stability of these trihalides depends on the cation as well as the trihalide anion. The assignment of a trihalide structure to these compounds was based on elemental analysis and on IR-and Raman spectroscopic evidence. Most stable are the tribromide and [1X2]° salts. During all reactions involving N-alkylamino-and N-cyclo-alkylaminotriphenylphosphonium halides and elemental halogens an N-halogenation of the cation was not observed. 
  Reference    (Z. Naturforsch. 38b, 103—107 [1983]; received September 20 1982) 
  Published    1983 
  Keywords    Halides, IR Spectra, Raman Spectra 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0103.pdf 
 Identifier    ZNB-1983-38b-0103 
 Volume    38 
3Author    M. Bobadilla, M. MoránRequires cookie*
 Title    Oxidative Addition of Pseudohalogen to [P(OPh)3]4Ni  
 Abstract    The title compound reacts with cyanogen halides, XCN (X = Br or I) to give the com-plexes L2(X)(CN)Ni (L = P(OPh)3, X = Br or I). The oxidative addition of (SCN)2 and (SeCN)2 to the same compound results in the formation of L2Ni(XCN)2 (X = S or Se). All the complexes have been characterized by elemental analysis, and IR, iH NMR and electronic spectra. 
  Reference    Z. Naturforsch. 38b, 1069—1071 (1983); received May 13 1983 
  Published    1983 
  Keywords    Pseudohalogens, IR Spectra, Nickel 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-1069.pdf 
 Identifier    ZNB-1983-38b-1069 
 Volume    38 
4Author    M-S Delgado, M-J Macazaga, J.R M AsaguerRequires cookie*
 Title    Oxidative Addition Reactions of P(CN)" P(NCO)3 and P(NCS), to (i/5-C5Me5 )Co(CO)2  
 Abstract    The phosphorus pseudohalogens P(CN)3, P(NCO)3 and P(NCS)3 react with (?/5-C5Me5)C o(C O)2 to give the complexes (?75-C;Me5)Co(CO)XPX2 (X = CN, NCO, NCS). All the compounds are characterized by elemental analysis, IR. electronic and 'H NMR spectra. 
  Reference    Z. Naturforsch. 39b, 142 (1984); received October 3 1983 
  Published    1984 
  Keywords    Phosphorus Pseudohalogens, IR spectra, Cobalt 
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 TEI-XML for    default:Reihe_B/39/ZNB-1984-39b-0142.pdf 
 Identifier    ZNB-1984-39b-0142 
 Volume    39 
5Author    Gerhard Beber, Jürgen Hanich, Kurt DehnickeRequires cookie*
 Title    Reaktionen von Yanadiumtetrachlorid mit Trithiazylchlorid Reactions of Vanadium Tetrachloride with Trithiazylchloride Vanadiumtrichloride-Thiazylchoride Adduct, Tetrachlorovanadate(III)-S 2 N 2  
  Reference    (Z. Naturforsch. 40b, 9—12 [1985]; eingegangen am 24. September 1984) 
  Published    1985 
  Keywords    Adduct, Preparation, IR Spectra 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0009.pdf 
 Identifier    ZNB-1985-40b-0009 
 Volume    40 
6Author    Bernhard Czeska, Kurt DehnickeRequires cookie*
 Title    [P(C 6 H 5 ) 4 ] 2 S 8 : Synthesis and IR Spectrum  
 Abstract    [P(C 6 H 5)4] 2 S g was prepared from Na 2 S 4 and PPh 4 Cl in ethanol solution and characterized by its IR spectrum. 
  Reference    (Z. Naturforsch. 40b, 120—121 [1985]; eingegangen am 28. September 1984) 
  Published    1985 
  Keywords    Tetraphenylphosphonium Octasulfide, Synthesis, IR Spectra 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-0120_n.pdf 
 Identifier    ZNB-1985-40b-0120_n 
 Volume    40 
7Author    H. Eribert, W. Adle, Kurt Dehnicke, D. Ieter FenskeRequires cookie*
 Title    (AsPh4)4[CrCl4(/J-N2S2)]4 * 8 CH2C12; Synthese, IR-Spektrum und Kristallstruktur (A sPh4)4[CrCl4(w-N2S2)]4 -8 CH 2C12; Synthesis, IR Spectrum and Crystal Structure  
 Abstract    Trithiazylchloride, (NSC1)3, reacts with metallic chrom ium, with chromium hexacarbonyl, with CrCl3-3 thf, as well as with chrom ium (VI) oxide to form mixtures, in which S4N 3®[CrCl4(N 2S2) ] 0 can be identified as the major product. This com pound reacts with tetraphenylarsonium chloride in dichlorom ethane to form the title com pound, which we have characterized by IR spectroscopy and an X-ray crystal structural analysis. (A sP h4)4[CrCl4(N 2S2)]4 -8 C H 2C12 crystallizes m onoclini-cally in the space group C 2 /c with four formula units per unit cell and with the follow ing lattice constants at —100 °C: a = 2146, b = 2033, c = 3137 pm; ß = 96.0° (9918 independent observed reflexions, R = 0.064). The com pound consists o f A sPh4® ions, tetrameric anions [CrCl4(N 2S2)]44e and included C H 2C12 m olecules. The chromium atom s of the anions occupy the corners o f a nearly ideal square; they are connected via the N -atom s o f planar N 2S2-rings, which are oriented perpendicularly to the Cr4-plane. The chromium atom s com plete their distorted octahedral coordination with four terminal chlorine atom s, the axial ones o f which form short Cl---S-contacts o f average 310 pm to the S-atom s o f the N 2S2-rings. 
  Reference    Z. Naturforsch. 40b, 1314—1319 (1985); eingegangen am 2. Mai 1985 
  Published    1985 
  Keywords    Trithiazylchloride, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/40/ZNB-1985-40b-1314.pdf 
 Identifier    ZNB-1985-40b-1314 
 Volume    40 
8Author    J. Fritze, W. PreetzRequires cookie*
 Title    c/osö-Halogenohydrohexaborate, III Schwingungsspektren der c/oso-Halogenohydrohexaborate X"B  
 Abstract    ~, n = 1-5; X = Cl, Br, I c/oso-Halogenohydrohexaborate, III Vibrational Spectra of the c/oso-Halogenohydrohexaborates X"B 6 H 6 _" 2_ , n = 1-5; X = Cl, Br, I The IR and Raman spectra of 20 different halogenohydrohexaborates, including pairs of geometric isomers of the series X"B 6 H 6 _ n :_ , X = Cl, Br, I; n = 1—5, have been assigned according to their point groups D 4h , C 4v , C 3v and C 2v determined previously by NMR studies. Due to weak coupling, the vibrations are treated separately to a first approximation in terms of internal B 6 -cage modes on one hand and modes of the substituents against the cage entity on the other hand. Disregarding the splitting by lowered symmetry, depending on the degree of halogenation, all internal modes of the B 6 cluster are observed at nearly unchanged positions in the range of 450—1250 cm -1 . The B 6 —X stretching vibrations, however, exhibit significant shifts to lower energy with increasing mass of substituents. 
  Reference    Z. Naturforsch. 42b, 293—300 (1987); eingegangen am 21. November 1986 
  Published    1987 
  Keywords    Halogenohydrohexaborates, IR Spectra, Raman Spectra 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0293.pdf 
 Identifier    ZNB-1987-42b-0293 
 Volume    42 
9Author    Kurt Dehnicke, Rainer LößbergRequires cookie*
 Title    Preparation and IR Spectrum of 0s04 * 2 SbCl5  
 Abstract    Osmiumtetroxide and antimony pentachloride form a donor acceptor complex, 0s04 • 2 SbCls. According to the IR spectrum the complex contains OsOSb bridges. With VCLj, TiCU, M0CI5 and osmiumtetroxide rapid ligand exchange reactions occur, forming VOCI3, TiOCl2 and several oxochlorides of molybdenum and OsCLi, respectively. 
  Reference    Z. Naturforsch. 35b, 1587—1588 (1980); eingegangen am 4. August 1980 
  Published    1980 
  Keywords    Preparation, IR Spectra, Osmiumtetroxide-Antimonypentachloride Donor-Acceptor Complex 
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 TEI-XML for    default:Reihe_B/35/ZNB-1980-35b-1587_n.pdf 
 Identifier    ZNB-1980-35b-1587_n 
 Volume    35 
10Author    HeribertW. Adle, Elke Conradi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von [W Cl3(N 3S2)(Pyridin)] Synthesis and Crystal Structure of [WCl3(N 3S2)(Pyridine)]  
 Abstract    1,1.1 -T richloro-1 -pyridine-cyclo-1 Ä6-tungsta-3.5-dithia-2,4, 
  Reference    Z. Naturforsch. 41b, 796—798 (1986); eingegangen am 14. Februar 1986 
  Published    1986 
  Keywords    6-triazine, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-0796_n.pdf 
 Identifier    ZNB-1986-41b-0796_n 
 Volume    41 
11Author    E. Kkehard Lindner, Petra NeeseRequires cookie*
 Title    Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, LII [1] Bindungs-und Strukturverhältnisse von Phosphidocobaltaten in Lösung und im festen Zustand Preparation and Properties of, and Reactions with, M etal-Containing Heterocycles, LII [1] Bonding and Structural Conditions of Phosphidocobaltates in Solution and in Solid State  
 Abstract    Reduction o f [(O C)3C oPPh2]" (la) with excess sodium granules affords [(O C)3CoPPh2]N a2 (3a) in solution as well as in solid state. H ow ever, in analogous reactions o f [(O C)3C oP R 2H ]2 (lb : R = C6H n ; lc : R = r-Bu) with excess sodium granules the m onovalent anionic com plexes [(O C)3C oP R 2H ]Na (2b, c) are obtained in TH F solution. 2 b , c cannot be isolated in solid state. A fter removal of TH F from their solutions the purified residues were identified by elem ental 
  Reference    Z. Naturforsch. 41b, 870 (1986); eingegangen am 26. Februar 1986 
  Published    1986 
  Keywords    Phosphidocobaltates, Structure, Reactivity, IR Spectra, N M R Spectra 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-0870.pdf 
 Identifier    ZNB-1986-41b-0870 
 Volume    41 
12Author    Bernd RebenstorfRequires cookie*
 Title    Über die Reaktion von Chromocen mit einem Co/Kieselgel-Träger On the Reaction of Chromocene with a Co/Silica Gel Support  
 Abstract    The IR spectra of the modified chromocene/Co/silica gel catalyst show a band at 3118 cm" 1 of the cyclopentadienyl ligand, which is shifted by —1-20 cm' 1 compared to the unmodified chromocene/silica gel catalyst. The comparably slow CO adsorption yields two bands at low Cr concentration (—0.1% Cr) at 2065 and 2022 cm" 1 and two more at higher Cr concentration (—1% Cr) at 2028 and 1961 cm -1 . Both band pairs are significantly different from that observed with the "normal" chromocene/silica gel catalyst at 2046 and 1974 cm -1 . No CO IR bands at low wavenumbers were observed with the modified catalyst. Polymerisation measurements showed a slightly lower concentration of catalytically active sites (35% of Cr) for the modified catalyst compared to the unmodified one (50%), while the poly-merisation activity decreased by a factor of four (Cr concentration: 0.083%). It was concluded that the surrounding of the dimeric surface site is changed by Co on the silica gel surface of the chromocen catalyst and that this change is important for the CO adsorption and the polymerisation activity. 
  Reference    Z. Naturforsch. 42b, 764—768 (1987); eingegangen am 18. Dezember 1986 
  Published    1987 
  Keywords    Silica Gel Cobalt(II), Chromocene, IR Spectra 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0764.pdf 
 Identifier    ZNB-1987-42b-0764 
 Volume    42 
13Author    Kay Jansen, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von (PPh4)2[Mo2(02C—Ph)4Cl4] * 2 CH2C12, einem Komplex mit Mo=Mo-Bindung Synthesis and Crystal Structure of (PPh4 )2 [Mo2 (0 2 C —Ph)4 Cl4] -2 CH 2 C12, a Complex with M o=M o Bonding  
 Abstract    The title com pound has been prepared from (PPh4)2[M o2(0 2C —Ph)4Cl2] and CC14 in C H 2C12 solution as moisture sensitive crystals, which are black in reflexion and yellow in transmission. (PPh4)2[M o2(0 2C —Ph)4Cl4] • 2 C H 2C12 was characterized by a X-ray crystal structure determ ination (7873 observed independent reflexions, R = 0.048). It crystallizes in the space group P 1 with one formula unit in the unit cell; the lattice constants are a = 1186.4; b = 1404.0; c = 1451.0 pm; a = 61.98°; ß = 78.91°; y = 78.26°. The structure consists o f PPh4® ions, C H 2C12 m olecules and centrosym m etric anions [M o2(0 2C —Ph)4Cl4]20 containing a molybdenum d3d3 unit with a relatively long M o = M o bond o f 249.6 pm. The M o= M o group is spanned in a chelate manner by four O atoms of two benzoate groups and by two further single O atoms o f two further benzoate groups. Two terminal Cl atom s on each Mo atom com plete the pentagonal bipyramidal coordination spheres about the Mo atoms. 
  Reference    Z. Naturforsch. 42b, 1097—1101 (1987); eingegangen am 2. März 1987 
  Published    1987 
  Keywords    Tetrabenzoato-tetrachloro-dim olybdate, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1097.pdf 
 Identifier    ZNB-1987-42b-1097 
 Volume    42 
14Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0094.pdf 
 Identifier    ZNB-1988-43b-0094 
 Volume    43 
15Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0138.pdf 
 Identifier    ZNB-1988-43b-0138 
 Volume    43 
16Author    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 
17Author    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 
18Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1319.pdf 
 Identifier    ZNB-1988-43b-1319 
 Volume    43 
19Author    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 
20Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1616.pdf 
 Identifier    ZNB-1988-43b-1616 
 Volume    43