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41Author    Jochen Jander, Alexander MaurerRequires cookie*
 Title    Untersuchungen an Stickstoff-Iod-Verbindungen, XVII [1] Weitere tertiäre N-Basen als Stabilisatoren des Iodonium-Kations und der Iodhalogenide Studies on Nitrogen-Iodine Compounds, XVII [1] Further Tertiary N-Bases as Stabilizers of the Iodonium Cation and Iodine Halides  
 Abstract    The preparation and properties of the new compounds [1(2,4 lutidine)2]N03, -C104, [1(2,6 lutidine)2]N03, -C104, [1(2,4,6 collidine)2]N03, -C104, [I(TEDA)2]N03, [I(quinu-clidine)2]SbCl6, quinuclidine • IBr, quinuclidine • IC1, quinuclidine • IClSbCls, TED A • I2, I2 • TEDA • I2, and C1I • TEDA • IC1 are reported. The molecular vibrations and force constants are compared to those of similar compounds previously prepared. 
  Reference    Z. Naturforsch. 33b, 1446—1451 (1978); eingegangen am 3. August 1978 
  Published    1978 
  Keywords    Bis-base-iodonium Salts, Mono-base-iodine Halides, Preparation, Properties, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/33/ZNB-1978-33b-1446.pdf 
 Identifier    ZNB-1978-33b-1446 
 Volume    33 
42Author    Axel Thiele, Joachim FuchsRequires cookie*
 Title    Struktur und Schwingungsspektren von Monomolybdaten und Monowolframaten organischer Kationen Structure and Vibrational Spectra of Monomolybdates and Monotungstates with Organic Cations  
 Abstract    The crystal structures of dicyclohexylammonium-monomolybdate dihydrate [(C6Hh)2NH2]2MO04 • 2 H2O, (I), cyclohexylammonium-monomolybdate, (C6HHNH3)2MO04, (II) and terf-butylammonium-monotungstate, (C4HgNH3)2W04, (III), were elucidated. In I the anion has nearly tetrahedral structure, in II one Mo-0 distance is significantly shorter than the other three, and in III all four W-0 distances are different. In spite of the variety of structures the following basic principles are recognizable: 1) Each hydrogen atom of the cationic amino groups as well as of the water of crystallization forms hydrogen bridges. 2) Never are oxygen atoms of the same M0O4 connected by these bridges, but always oxygen atoms of neighbouring M0O4 units. 3) From an oxygen atom emanate either two or no hydrogen bridge. For the investigated molybdates (tungstates) there are in all instances isomorphous tungstates (molybdates). The number and position of the vibrational bands is in good agreement with the observed anion symmetry Td, C3V and Ci, respectively. 
  Reference    Z. Naturforsch. 34b, 145—154 (1979); eingegangen am 23. Oktober 1978 
  Published    1979 
  Keywords    Monomolybdates, Monotungstates, Organic Cations, Properties, X-ray, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/34/ZNB-1979-34b-0145.pdf 
 Identifier    ZNB-1979-34b-0145 
 Volume    34 
43Author    Jochen Eilermann, Martin LietzRequires cookie*
 Title    Chemie polyfunktioneller Liganden, 67 [1]  
 Abstract    Die Darstellung von l.l.l-Tris(dichlorarsinomethyl)ethan, Ethan-l.l.l-tris(methylarsonsäure), 1.1.1-Tris (arsinomethyl)ethan und einem neuen Organocyclotriarsan Chemistry of Polyfunctional Ligands, 67 [1] The Preparation of l.l.l-Tris(dichloroarsinomethyl)ethane, Ethane-l.l.l-tris(methylarsonic acid), l.l.l-Tris(arsinomethyl)ethane and of a New Organocyclotriarsane l,l,l-Tris(dichlorarsinomethyl)ethane, CH3C(CH2AsCl2)3 (5) can be obtained in the reaction of CH3C(CH2AsNC6H4CH3)3 (4) with gaseous HCl. The heteroadamantane CH3C(CH2AsO)3 (6) reacts with AsCl3 or PC13 yielding also 5. CH3C(CH2AsO)3, CH3C(CH2AsS)3 and CH3C(CH2AsI 2)3 are oxidized with H202 to give CH3C[CH2As(0)(0H)2]3 (7) and CH3C[CH2As(0)(0H)2]3 • H20 (7 a). CH3C(CH2AsI2)3 and C(CH2AsI2)4 can be reduced with LiAlH4 to give CH3C(CH2AsH2)3 (9) and C(CH2AsH2)4 (12). Oxidation of 9 and 12 leads to the cyclotriarsane compounds CH3C(CH2As)3 (10) and H2AsCH2C(CH2As)3 (13). 
  Reference    (Z. Naturforsch. 37b, 73—80 [1982]; eingegangen am 29. Juni/21. September 1981) 
  Published    1982 
  Keywords    Arsenic Compounds, Organocyclotriarsane, Vibrational Spectra, *H NMR Spectra, Mass Spectra 
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 TEI-XML for    default:Reihe_B/37/ZNB-1982-37b-0073.pdf 
 Identifier    ZNB-1982-37b-0073 
 Volume    37 
44Author    Karl Schlosser, Helge WillnerRequires cookie*
 Title    Photochemisches Verhalten von (CF3S)2CS in Inertgasmatrix Photochemical Behavior of (CFsS^CS in Rare Gas Matrix  
 Abstract    Infrared spectra have been recorded of (CFsS^CS in the gas and solid phase as well as isolated in noble gas matrix; the Raman spectra of the liquid have also been taken. The analyses of the spectra show that this compound consists of a complex mixture of con-formers. By photolysis in a matrix with light of wavelength > 300 nm the distribution of the conformers changes and with light of wavelength > 530 nm this change can be reversed. The threshold for photochemical decomposition in the matrix is about 300 nm. The decomposition products consist of an equimolar mixture of CF3SCF3 and CS2. 
  Reference    Z. Naturforsch. 38b, 161—167 (1983); eingegangen am 23. September/15. November 1982 
  Published    1983 
  Keywords    Bis(trifluormethyl)trithiocarbonate, Vibrational Spectra, Conformers, Rare Gas Matrix, Photochemical Behaviour 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0161.pdf 
 Identifier    ZNB-1983-38b-0161 
 Volume    38 
45Author    Umlagerung Synthese, Eigenschaften Diphenylphosphinosubstituierter Uracile, Jochen Ellermann, AlfonsA M DemuthRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 74 [1] [1] Synthesis, Rearrangement and Properties of Diphenylphosphino Substituted Uracils  
 Abstract    5-Bromo-uracil (2) with chloro-diphenylphosphine and triethylamine gives 5-bromo-N(1),N(3)-bis(diphenylphosphino)-uracil (3). In moist acetone, 3 is hydrolyzed to 5-bromo-N(l)-diphenylphosphino-uracil (4). 3 reacts with n-butyllithium under rearrangement and, with HCl, under elimination of a PPh2-group, forms C(5)-diphenylphosphino-uracil (7 a). Recrystallization of 7 a from ethanol yields the ethanol-1:1-adduct 7 b. Heating of 7 a in dimethylsulfoxide with D20 yields the N(l),N(3)-dideutero-C(5)-diphenylphosphino-uracil (7 c). All compounds were characterized by infrared, Raman, iH, 31 P NMR and mass spectra. 7 a shows a very small antitumor activity. 
  Reference    Z. Naturforsch. 38b, 1165—1172 (1983); eingegangen am 19. Mai 1983 
  Published    1983 
  Keywords    Diphenylphosphino Substituted Uracils, Rearrangement, NMR Spectra, Vibrational Spectra, Mass Spectra 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-1165.pdf 
 Identifier    ZNB-1983-38b-1165 
 Volume    38 
46Author    Ralf Steudel, Jürgen Steidel, Richard ReinhardtRequires cookie*
 Title    X-Ray Structural Analyses of Cyclodecasulfur (S10) and of a Cyclohexasulfur-Cyclodecasulfur Molecular Addition Compound (S6 * S10) [1]  
 Abstract    Low temperature X-ray structural analyses of monoclinic single crystals of Sio and Sö • Sio (prepared from the components) show that the cyclic Sio molecule exhibits the same D2 conformation in both compounds with bond distances between 203.3 and 208.0pm, bond angles (a) between 103 and 111°, and torsional angles (r) between 73 and 124°. The Sß molecule (site symmetry Ci) in Sö • Sio is very similar to the one in pure Sö (dss = 206.2 pm, a= 103°, r = 74°). All intermolecular interactions are of van-der-Waals type. The Raman spectrum of S6 • Sio can be explained by a superposition of the Se and Sio spectra. 
  Reference    Z. Naturforsch. 38b, 1548—1556 (1983); received August 11 1983 
  Published    1983 
  Keywords    Elemental Sulfur, Sulfur Rings, Molecular Structure, Crystal Structure, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-1548.pdf 
 Identifier    ZNB-1983-38b-1548 
 Volume    38 
47Author    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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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1305.pdf 
 Identifier    ZNB-1991-46b-1305 
 Volume    46 
48Author    M. =. Re, Tc, X. =. Ci, BrJ. Skowronek, W. PreetzRequires cookie*
 Title    Schwingungsspektren und Normalkoordinatenanalyse der Acetatohalogenodimetallate M 2( 0 2CCH3)4X2, M = Re, Tc; X = CI, Br Vibrational Spectra and Norm al Coordinate Analysis of Acetatohalogenodim etalates M 2( 0 2C CH 3)4X  
 Abstract    The orange-red Tc2(0 2C C H 3)4Br2 has been prepared for the first time by reaction of [Tc2Brg]2_ with glacial acetic acid and acetic anhydride. The IR and R am an spectra have been recorded at 80 K and are compared with those of the analogous com pounds Tc2(0 2CC H 3)4C12, Re2(0 2C C H 3)4Cl2 and Re2(0 2CC H 3)4Br2. The assignment according to the point group D 4h is supported by normal coordinate analysis based on a general valence force field. The quadruple M -M bond is stabilized by the bridging acetato and destabilized by the axial halogeno ligands. The valence force constants fd(MM) are determined to 3,96-4,08 mdyn/A. The inter­ action constants fdd(M M /M X), fdd(M M /M O) and fJM M /M M O) are ab o u t three times high­ er for the technetates as compared with the rhenates. The stronger interaction between oppo­ site bonds in the equatorial ligand sphere is revealed by the stretching interaction constants d d '' which are about two times higher than fdd for M -O bonds at right angles. The strong coupling of the ring co-ordinates implies extensive mixing of the M -O valence and deform ation modes. The electronic spectra of Tc2(0 2CC H 3)4X, agree with those of the corresponding Re com ­ pounds. 
  Reference    Z. Naturforsch. 47b, 482—490 (1992); eingegangen am 10. Oktober 1991 
  Published    1992 
  Keywords    Tetraacetatodihalogenodirhenates, Tetraacetatodihalogenoditechnetates, Vibrational Spectra, UV-Vis Spectra, Normal Coordinate Analysis 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0482.pdf 
 Identifier    ZNB-1992-47b-0482 
 Volume    47 
49Author    Klaus-Jürgen Range, Peter Rögner, A. Nton, M. Heyns, LindaC. PrinslooRequires cookie*
 Title    An X-Ray, Raman and IR Study of a-C sR e04, the High-Temperature Modification of Cesium Perrhenate  
 Abstract    Cesium perrhenate undergoes a reversible phase transition from the orthorhom bic room-temperature phase (/?-CsRe04, space group Pnma) to a tetragonal high-temperature phase (a -C sR e 0 4). The space group o f a -C sR e 0 4 was unam biguously confirmed by high-tempera-ture X-ray diffraction to be 14 Jamd in contrast to the earlier literature, in which space group 14 Ja (and hence, a scheelite type structure) was assumed for a -C sR e 0 4. From a data set ob­ tained at 468 K the crystal structure o f a -C sR e 0 4 (a = 5.9607(4), c = 14.446(1)Ä, Z = 4) was refined to R = 0.032, Rw = 0.029 using anisotropic displacement factors. In the vibrational spectra not all o f the predicted com ponents for /?-C sR e04 could be con­ firmed by the experiments, but for a -C sR e 0 4 very good agreement was obtained between the predicted and observed bands. The fact that v2 at ~ 3 0 0 cm "' is not observed in the IR spectra o f a -C sR e 0 4 confirms the space group 14Jamd, since, under 14,/a symmetry, this band is allowed. The structure o f a -C sR e 0 4 consists o f isolated R e 0 4 tetrahedra which are linked together by cesium atoms. The relationships between the scheelite, a -C sR e 0 4 and /?-C sR e04 structural types are discussed. 
  Reference    Z. Naturforsch. 47b, 1513—1520 (1992); received June 15 1992 
  Published    1992 
  Keywords    Cesium Perrhenate, High-Temperature M odification, Crystal Structure, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1513.pdf 
 Identifier    ZNB-1992-47b-1513 
 Volume    47 
50Author    Chrystel Hagen, Hanns-D Ieter AmbergerRequires cookie*
 Title    Zur Elektronenstruktur hochsymmetrischer Verbindungen der /-Elemente, XXV.III) Single Crystals for Chemical Syntheses and Physical Investigations  
 Abstract    Züchtung hochreiner Tris[bis(trimethylsilyl)amido]lanthanoid(III)-Einkristalle für chemische Synthesen und physikalische Untersuchungen The Electronic Structure o f Highly Symmetrical Compounds o f the /-Elem ents, XXV. Grow th of U ltrapure Tris[bis(trimethylsilyl)amido]lanthanide(Tris[bis(trimethylsilyl)amido]lanthanide(III 
  Reference    Z. Naturforsch. 48b, 1365—1371 (1993); eingegangen am 17. Juni 1993 
  Published    1993 
  Keywords    ) Complexes, Large Oriented Single Crystals, Optical Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-1365.pdf 
 Identifier    ZNB-1993-48b-1365 
 Volume    48 
51Author    Birgit Bäck, H. An, S. PreutRequires cookie*
 Title    Uber die Reaktionen von Molekülen  
 Abstract    (R2CS)2 (R = CF3, CI) und C12CS mit XeF+MF6-(M = As, Sb) und Kristallstruktur von (CF3)2CSC(CF3)2SF+SbF6-[1] O n th e R eactions of M olecules (R 2C S)2 (R = C F 3, Cl) and C12CS with X eF +M F6_ (M = As, Sb) and C rystal Structure of (C F3)2C SC (C F3)2SF+SbF6~ [1] R olf M inkwitz XeF+MF6_ (M = As, Sb) reacts with ((CF3)2CS)2 and C12CS to form the corresponding monofluorinated sulfonium hexafluorometalates. The salts have been characterized by vibra­ tional and 19F NMR spectroscopic measurements. (CF3)2CSC(CF3)2SF+SbF6^ crystallizes in the monoclinic space group C2/c with a =o 14.791(10), b = 11.093(6), c -10.356(6)Ä, ß -119.83° and Z = 4. With a value of 1.51(1) A d (S -F) is comparable to the SF-bond distance in (CF3)(C1)CSC(CF3)(C1)SF+AsF6-. 
  Reference    Z. Naturforsch. 49b, 881—888 (1994); eingegangen am 10. November 1993 
  Published    1994 
  Keywords    Monofluorosulfonium Salts, Preparation, Vibrational Spectra, 19F NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0881.pdf 
 Identifier    ZNB-1994-49b-0881 
 Volume    49 
52Author    W. Lübbe, A. Franken, W. PreetzRequires cookie*
 Title    Darstellung, n B-, 13C-, 'H-NMR-und Schwingungsspektren  
 Abstract    von 1.2-Trimethylenpentahydro-closo-Hexaborat(l -) , c i s -[B6H5(CH2)3]" und 1.2-TetramethyIenpentahydro-closo-Hexaborat(l-), cjs-[B6H5(CH2)4]_ sowie Kristallstrukturen von [P(C6H5)4][B6H5(CH2)3] und [P(C6H5)4][B6H5(CH2)4] Preparation, n B, 13C, 'H NMR and Vibrational Spectra of 1.2-Trim ethylenepentahydro-closo-hexaborate(l-), ds-[B 6H 5(C H 2)3]_, and 1.2-Tetram ethylenepentahydro-closo-hexaborate(l-), ds-[B 6H 5(CH 2)4]~, and the Crystal Structures of [P(C6H 5)4][B6H 5(CH 2)3] and [P(C6H 5)4][B6H 5(C H 2)4] 1.2-Trimethylenepentahydro-closo-hexaborate(l -) , 1.2-Tetram ethylenepentahydro-closo-hexaborate( 
  Reference    Z. Naturforsch. 49b, 1115—1122 (1994); eingegangen am 17. Januar 1994 
  Published    1994 
  Keywords    ), Crystal Structures, 'H NM R Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1115.pdf 
 Identifier    ZNB-1994-49b-1115 
 Volume    49 
53Author    H. Arald Hillebrecht, G.Erhard Thiele, Alrik Koppenhöfer, Heinrich VahrenkampRequires cookie*
 Title    Kristallstruktur und Schwingungsspektren von Zn(NH 3)4(C104)2 Crystal Structure and Vibrational Spectra of Zn(N H 3)4(C104)2  
 Abstract    The title compound Z n (N H 3)4(C104)2 crystallizes in the space group F 43m with a = 10.240(1) A. The crystal structure consists of tetrahedral Z n (N H 3)4 cations and two non­ equivalent C 104 anions with crystallographic Td symmetry. The complex ions constitute an arrangement which is known from the Zintl phase M gAgAs. The Z n(N H 3)4 cations are ccp packed with perchlorate anions in octahedral and tetrahedral voids. W hereas the C 104 ions centered at tetrahedral holes do not interact with the other lattice components, the perchlo­ rate ions in the octahedral voids are connected with the ammine ligands by a hydrogen bonded three-dimensional network involving all their N, H, and O atoms. The repeating unit of this network is a N40 4(m-H)12 cube with N -H = 1.19(2)A and O -H = 1.98(2)A . Raman and IR spectra were recorded between 150 and 4000 cm -1. A ll the expected internal m odes of the com plex ions could be detected and assigned. The crystallographically different C 104 anions have nearly the same vibrational spectra, only a slight splitting o f two IR m odes is observed. 
  Reference    Z. Naturforsch. 49b, 1163—1168 (1994); eingegangen am 25. März 1994 
  Published    1994 
  Keywords    Zinc Am m ine, Perchlorate, Cubic Structure, Hydrogen Bonds, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1163.pdf 
 Identifier    ZNB-1994-49b-1163 
 Volume    49 
54Author    A. Franken, W. PreetzRequires cookie*
 Title    Darstellung, n B-NMR-und Schwingungsspektren  
 Abstract    von Am inohexahydro-closo-hexaborat(l-), [B6H6(NH2)]~ sowie Kristallstruktur von Cs[B6H6(NH2)]*H 20 P rep aratio n , n B N M R and V ibrational Spectra of A m in o h e x a h y d ro -c lo so -h ex a b o ra te (l-), [B6H 6(N H 2)]' , and the C rystal S tructure of Cs[B6H 6(N H 2)] • H 20 By reduction of [B6H5(N0 2)]2_ with Fe2+ in aqueous alkaline solution [B6H6(NH2)]~ is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] H20 has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) Ä, ß = 100.168(6)°. The UB NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N -H , B -H and B6 vibrations. 
  Reference    (Z. Naturforsch. 50b, 11—14 [1995]; eingegangen am 9. August 1994) 
  Published    1995 
  Keywords    Aminohexahydro-closo-hexaborate(l-), Crystal Structure, UB NMR Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0011.pdf 
 Identifier    ZNB-1995-50b-0011 
 Volume    50 
55Author    Abdel-Fattah Shihada, Frank WellerbRequires cookie*
 Title    Synthesis, Vibrational Spectra, Mass Spectrum and Crystal Structure of Tri-n-butyltin Diphenylphosphinate (n-Bu)3S n 0 2PPh2  
 Abstract    Tri-/?-butyltin diphenylphosphinate (/?-Bu)3S n 0 2PPh2 has been synthesized by the reaction o f («-B u 3Sn)20 with Ph2POCl in toluene. An X-ray diffraction study of (/?-Bu3) S n 0 2PPh2 shows that the structure is polymeric and consists of helical chains in which (/7-Bu)3Sn groups are linked by O-P-O bridges. The geometry about tin is trigonal bipyramidal, with «-butyl groups in equatorial positions and an axial O -S n -O angle of 176.2 (2)°. IR and Raman spectra of («-B u)3SnÖ2PPh2 are given and assigned. The mass spectrum is reported and discussed. 
  Reference    Z. Naturforsch. 50b, 1343—1347 (1995); received D ecem ber 12 1994 
  Published    1995 
  Keywords    Crystal Structure, Vibrational Spectra, Mass Spectrum, Tri-n-butyltin Diphenylphosphinate 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1343.pdf 
 Identifier    ZNB-1995-50b-1343 
 Volume    50 
56Author    G. O. Stendorp3, O. Tterb, H. HomRequires cookie*
 Title    Syntheses and Properties of Cerium Diphthalocyanines in High Oxidation States; Crystal Structure of [C e(Pc)2](BF4) 0.33  
 Abstract    Ring oxidized green Cerium(IV)diphthalocyanines, [Ce(Pc)2]X (X = (poly)halide, N 0 3_) are prepared by chemical oxidation of ("Bu4N)[Ce(Pc2~)2] with the corresponding halogen in solution or of solid [Ce(Pc2_)2] with aqueous HNO> Electrochemical oxidation of ("Bu4N)[Ce(Pc2_)2] in solution in the presence of ("Bu4N)BF4 yields [Ce(Pc)2](BF4)0.;p, which crystallizes in the tetragonal space group P4/nnc (a, b = 19.643(3) A, c = 6.525(3) A, Z = 2). The CeIV ion is eightfold coordinated by the isoindole N atoms (Niso) of the two staggered (ca. 41°), slightly distorted Pc ligands. The "[Ce(Pc)2]<)33+" subunits are arranged in infinite columns along [001] with the Ce atoms statistically disordered over two positions and C e -N iso bond lengths of 2.45(1) and 2.69(1) A, respectively The UV-VIS spectrum is dominated by the transitions of the Pc2-ligand at ca. 15,000 (B band), 30,000 and 36,000 cm -1 (Q, N region). A low energy ("metallic") band at ca. 2800 cm -1 typical for partially oxidized systems is present. The UV-VIS-NIR spectrum of [Ce(Pc)2]N 0 3 indicates a cofacial Pc2" -P c -complex. In addition to the jt-jz' transitions of the Pc2-moiety at ca. 14,000, 30,000 and 36,000 cm-1, the Ch transition of the Pc-ring is observed at ca. 19,200 cm -1 and the typical N IR band at 6380 cm -1. Oxidation of a thin film of (PNP)[Ce(Pc2_)2] with dry Br2/ N2 gas yields purple [Ce(Pc_)2]B rv, whose UV-VIS-NIR spectrum shows the diagnostic fea­ tures of dimeric Pc~ radicals with intense bands at ca. 14,000 and 18,000 cm -1 assigned as B and Qi bands, respectively. A t ca. 9000 cm 1 the typical Q D absorption is observed. The vibrational spectra are dom inated by the transitions of the Pc-ligand at 1305/1445 cm -1 (IR) and 560/1120/1172/1591 cm-1 (resonance Raman). Excitation with 1064 nm strongly enhances the sym. C e -N stretch at 163 c m '1. 
  Reference    Z. Naturforsch. 51b, 567—573 (1996); received September 14 1995 
  Published    1996 
  Keywords    Diphthalocyanines, Cerium Compounds, Crystal Structure, UV-VIS-NIR Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0567.pdf 
 Identifier    ZNB-1996-51b-0567 
 Volume    51 
57Author    W. Lübbe, W. PreetzRequires cookie*
 Title    undm-[(w-C4H9)4N][B6H5(CH2)2C6H4]  
 Abstract    Preparation, n B, 13C, 'H NM R Spectra and Vibrational Spectra o f 1,2-Xylylene-pentahydro-c/oso-hexaborate, cw-[B6H5(CH2)2C6H4]_ , and the Crystal Structures o f c/s-[P(C6H5)4][B 6H5(CIL,)2C6H4] and c/s-[(n-C4H9)4N ][B 6H5(CH2)2C6H4] 1,2-Xylylene-pentahydro-c/oso-hexaborat(1 -), ' By reaction of [B6H6]2-with u>,u/-dibromo-o-xylene in acetonitrile the 1,2-xylylene-pentahydro-c/oso-hexaborat, ds-[B 6H5(CH2)2C6H4]_ , is formed. The new ansa compound has been separated from excess [B6H6]2-and other reaction products by ion exchange chromatogra­ phy on diethylaminoethyl cellulose. The crystal structures of c/s-[P(C6H5)4][B6H5(CH2)2C6H4] (I) and as-[(n-C4H9)4N][B6H5(CH2)2C6H4] (II) have been determined by single crystal X-ray diffraction analysis: I is monoclinic, space group P 2 \/n with a = 13.715(5), b = 11.118(1) and c = 19.702(2) A, ß = 103.47(2)°; II is orthorhombic with a = 10.204(7), b = 13.352(4) and c = 20.824(8) A. The "B NMR spectrum confirms the structure with a hetero disubstituted octahedral B6 cage with local C2v symmetry. The l3C and 'H NMR spectra have been assigned in term of such a configuration. The IR and Raman spectra exhibit characteristic CH, BH, BC, B6 and arene vibrations. 
  Reference    Z. Naturforsch. 51b, 691—697 (1996); eingegangen am 25. August 1995 
  Published    1996 
  Keywords    H NMR Spectra, Vibrational Spectra, 13C NMR Spectra, 11B NMR Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0691.pdf 
 Identifier    ZNB-1996-51b-0691 
 Volume    51 
58Author    ]. C. Nachtigal, W. PreetzRequires cookie*
 Title    Darstellung, n B-NMR  
 Abstract    , Schwingungsspektren und Kristallstruktur von Bis(tetraphenylphosphonium)-2-[2-(2-pyridyl-amino)-pyrid-5-yl]-c/oso-decaborat, [P(C6H5)4]2[2-{2-(2-(C5H4N)-NH)-(C5H3N)-5}B10H9] Preparation, 11B NMR, Vibrational Sprectra and Crystal Structure of Bis(tetraphenylphosphonium) 2-[2-(2-Pyridyl-amino)-pyrid-5-yl]-c/fxw-decaborate, [P(C6H5)4]2 [2 2-[2-(2-Pyridyl-am ino)-pyrid-5 -yl]-c7r« 0-decaborate( 
  Reference    Z. Naturforsch. 51b, 1559—1562 (1996); eingegangen am 29. Mai 1996 
  Published    1996 
  Keywords    ), Crystal Structure, n B NMR Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1559.pdf 
 Identifier    ZNB-1996-51b-1559 
 Volume    51 
59Author    X. =. Cl, I. V. Br, W. Lorenzen, PreetzRequires cookie*
 Title    Kristallstrukturen von Oi-Bu4N)  
 Abstract    [B6C16], (w-Bu4N)[B6Br6] und (Ph3P=N=PPh3)[B6I6] sowie Schwingungsspektren und Normal-koordinatenanalyse der Hexahalogeno-c/osö-Hexaboratradikal-anionen [B6X6]~, X = Cl, Br, I Crystal Structures of («-Bu4N)[B6C16], (rc-Bu4N)[B6Br6], and (Ph3P=N=PPh3)[B6I6], and Vibrational Spectra and Normal Coordinate Analysis of the Hexahalogeno-c/oso-hexaborate Radical Anions [B6X6]-, Oxidation of hexahalogeno-c/oso-hexaborates [B6X6]2_, X = Cl, Br, I, with (NH4)2[Ce(N03)6] in ethanol yields coloured radical ions [B6X6]~. X-ray structure determina­ tions have been performed on single crystals of («-Bu4N)[B6Cl6] (1) (monoclinic, space group P2,/c,a = 13.144(2),6 = 12.594(2),c = 17.688(5) A,ß = 107.29(2)°,Z=4),(«-B u4N)[B6Br6] (2) (monoclinic, space group P2,/c, a = 13.529(5), b = 13.096(5), c = 17.863(5) Ä, ß = 107.20(5)°, Z = 4) and (Ph3P=N=PPh3)[B6I6] (3) (triclinic, space group P I, a = 9.3137(8), b = 10.6988(10), c = 11.8760 A, a = 102.220(7), ß = 99.34J(8), 7 = 96.030(7)°, Z = 1). The average B-B distan­ ces are nearly equal (1.733 Ä (1), 1.728 A (2), 1.728 A (3)) while the B-X distances increase (1.762 A (1), 1.912 A (2), 2.120 A (3)). Using the molecular parameters, normal coordinate analyses have been performed and a good agreement of observed and calculated frequencies of 11B and 1 'B labelled derivatives has been achieved. The valence force constants fd(BB) and fd(BX) of [B6X6]" are 1.17 and 4.17 (X = Cl), 1.18 and 3.34 (Br) and 1.18 and 2.60 mdyn/A (I), respectively. 
  Reference    Z. Naturforsch. 52b, 565—572 (1997); eingegangen am 19. Februar 1997 
  Published    1997 
  Keywords    Hexahalogenohexaborates( 1 -), Crystal Structure, Vibrational Spectra, Normal Coordinate Analysis 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0565.pdf 
 Identifier    ZNB-1997-52b-0565 
 Volume    52 
60Author    T. Koch, W. PreetzRequires cookie*
 Title    Darstellung, n B  
 Abstract    ,13 C -,1 H-NMR-und Schwingungsspektren von Phenylundecahydro-c/oso-dodecaborat(2-) sowie Kristallstruktur von [As(C6H5)4]2[(C6H5)B12H n ] Preparation, n B, 13C, 'H NMR and Vibrational Spectra of Phenylundecahydro-c/oso-dodecaborate(2-) and Crystal Structure o f [As(C6H5)4]2[(C6H5)B 12H n ] 
  Reference    Z. Naturforsch. 52b, 935—938 (1997); eingegangen am 2. Mai 1997 
  Published    1997 
  Keywords    Phenylundecahydro-c/oso-dodecaborate(2-), Crystal Structure, 'H NMR Spectra, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0935.pdf 
 Identifier    ZNB-1997-52b-0935 
 Volume    52