| 41 | Author
| Jochen Jander, Alexander Maurer | Requires 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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| default:Reihe_B/33/ZNB-1978-33b-1446.pdf | | | Identifier
| ZNB-1978-33b-1446 | | | Volume
| 33 | |
42 | Author
| Axel Thiele, Joachim Fuchs | Requires 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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| default:Reihe_B/34/ZNB-1979-34b-0145.pdf | | | Identifier
| ZNB-1979-34b-0145 | | | Volume
| 34 | |
43 | Author
| Jochen Eilermann, Martin Lietz | Requires 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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| default:Reihe_B/37/ZNB-1982-37b-0073.pdf | | | Identifier
| ZNB-1982-37b-0073 | | | Volume
| 37 | |
45 | Author
| Umlagerung Synthese, Eigenschaften Diphenylphosphinosubstituierter Uracile, Jochen Ellermann, AlfonsA M Demuth | Requires 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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| default:Reihe_B/38/ZNB-1983-38b-1165.pdf | | | Identifier
| ZNB-1983-38b-1165 | | | Volume
| 38 | |
46 | Author
| Ralf Steudel, Jürgen Steidel, Richard Reinhardt | Requires 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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| default:Reihe_B/38/ZNB-1983-38b-1548.pdf | | | Identifier
| ZNB-1983-38b-1548 | | | Volume
| 38 | |
47 | Author
| J. Skowronek, W. Preetz, S. M. Jessen | Requires 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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| default:Reihe_B/46/ZNB-1991-46b-1305.pdf | | | Identifier
| ZNB-1991-46b-1305 | | | Volume
| 46 | |
48 | Author
| M. =. Re, Tc, X. =. Ci, BrJ. Skowronek, W. Preetz | Requires 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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| default:Reihe_B/47/ZNB-1992-47b-0482.pdf | | | Identifier
| ZNB-1992-47b-0482 | | | Volume
| 47 | |
49 | Author
| Klaus-Jürgen Range, Peter Rögner, A. Nton, M. Heyns, LindaC. Prinsloo | Requires 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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| default:Reihe_B/47/ZNB-1992-47b-1513.pdf | | | Identifier
| ZNB-1992-47b-1513 | | | Volume
| 47 | |
51 | Author
| Birgit Bäck, H. An, S. Preut | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-0881.pdf | | | Identifier
| ZNB-1994-49b-0881 | | | Volume
| 49 | |
52 | Author
| W. Lübbe, A. Franken, W. Preetz | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1115.pdf | | | Identifier
| ZNB-1994-49b-1115 | | | Volume
| 49 | |
53 | Author
| H. Arald Hillebrecht, G.Erhard Thiele, Alrik Koppenhöfer, Heinrich Vahrenkamp | Requires 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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| default:Reihe_B/49/ZNB-1994-49b-1163.pdf | | | Identifier
| ZNB-1994-49b-1163 | | | Volume
| 49 | |
54 | Author
| A. Franken, W. Preetz | Requires 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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| default:Reihe_B/50/ZNB-1995-50b-0011.pdf | | | Identifier
| ZNB-1995-50b-0011 | | | Volume
| 50 | |
56 | Author
| G. O. Stendorp3, O. Tterb, H. Hom | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0567.pdf | | | Identifier
| ZNB-1996-51b-0567 | | | Volume
| 51 | |
57 | Author
| W. Lübbe, W. Preetz | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-0691.pdf | | | Identifier
| ZNB-1996-51b-0691 | | | Volume
| 51 | |
58 | Author
| ]. C. Nachtigal, W. Preetz | Requires 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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| default:Reihe_B/51/ZNB-1996-51b-1559.pdf | | | Identifier
| ZNB-1996-51b-1559 | | | Volume
| 51 | |
59 | Author
| X. =. Cl, I. V. Br, W. Lorenzen, Preetz | Requires 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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| default:Reihe_B/52/ZNB-1997-52b-0565.pdf | | | Identifier
| ZNB-1997-52b-0565 | | | Volume
| 52 | |
60 | Author
| T. Koch, W. Preetz | Requires 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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| default:Reihe_B/52/ZNB-1997-52b-0935.pdf | | | Identifier
| ZNB-1997-52b-0935 | | | Volume
| 52 | |
|