| | 101 | Author
| H. Einer, Homborg | Requires cookie* | | | Title
| Inin -Phthalocyanine: Darstellung, Eigenschaften und Kristallstruktur von £-Bis(triphenylphosphin)iminium-as-di(cyanato(N))phthalocyaninato- (2-)indat(III)  | | | | Abstract
| In111 Phthalocyanines: Synthesis, Properties and Crystal Structure of Z?-Bis(triphenylphosphine)iminium c/5-D i(cyanato(N))phthalocyaninato(2-)indate(III) B arbara Aßm ann, A ndreas Franken, [In(Cl)Pc2~] reacts with bis(triphenylphosphine)iminium cyanate ((PNP)OCN) in dichlo-romethane to yield green-blue *(PNP) [In(NCO)2Pc2_] • CH2C12, which crystallizes in the triclinic space group Pi (No. 2) with Z = 2. The two cyanato(N) ligands are in a mutually cis coordination (Z (NNCO-In -N NCO) = 84.2(3)°). The In atom is displaced out of the plane of the four N,.vo atoms towards the two cyanato(N) ligands (d(In-Ct(N,JO)4) = 0.988 A). The average In-N NC0 and In-N,.so bond distances are 2.16(1) and 2.216(8) A, respectively. The NNco-In -NNCO moiety deviates by ~ 4° from the staggered conformation relative to the In-(N,,")4 sceleton. Though the cyanato(N) ligands are essentially linear, there are different In-N -C angles (164.4(9) and 147.1(8)°) probably due to crystal packing effects. The Pc2~ ligand is distorted in an asymmetrically convex manner. The PNP cation adopts the bent conformation (Z(P-N(K)-P) = 143.5(6)°). The cyclic voltammogram shows three electrode processes, which are assigned to the redox pairs: Pc ~/Pc2~ (-0.87 V) < In'/In111 (-0.63 V) < Pc~_ /Pc~ (0.69 V). The UV-VIS-NIR spectra and the vibrational spectra are discussed. | | | |
Reference
| Z. Naturforsch. 51b, 325—332 (1996); eingegangen am 21. August 1995 | | | |
Published
| 1996 | | | |
Keywords
| Indium(III) Phthalocyanines, Cyanato(N) Complex, Cyclic Voltammetry, Crystal Structure, Optical and Vibrational Spectra | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0325.pdf | | | | Identifier
| ZNB-1996-51b-0325 | | | | Volume
| 51 | |
| 102 | Author
| W. Lübbe, W. Preetz | Requires cookie* | | | Title
| Darstellung, n B -,13C -,1 H-NMR-und Schwingungsspektren von ja-Dimethylen-bis | | | | Abstract
| hexahydro-c/oso-hexaborat, [B6H6(CH2)2B6H6]2', sowie Kristallstrukturen von [As(C6H5)4]2[B6H6(CH2)2B6H6] [(CH3)2CO] und [P(C6H5)4]2[B6H6(CH2)2B6H6][C 2H5OH] Preparation, " B , 13C, 'H NM R and Vibrational Spectra of /i-Dimethylene-bis-hexahydro-c/oso-hexaborate, [BeHöCCI^hBöHö]2" , and the Crystal Structures o f [As(C6H5)4]t[B 6H6(CH2)2B 6H6] [(CH3)?CO] and [P(C6H5)4]2 [B6H6(CH2)2B6H6] • [C2H5OH] ^-Dimethylene-bis-hexahydro-c/as'o-hexaborate(2- By reaction of [B6H6]2~ with dibromoethane in acetonitrile /j-dimethylene-bis-hexa-hydro-c/oso-hexaborate(2-), JBfiHötCfLbBfcHö]2 -, is formed. The compound was sepa rated from excess [B6H6]'_ by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of [AstCfiH.^MBöHötCHbhBöHftl-IXCI-L^CO] (I) and [P(Cf,H5)4]2[BftH^CHT^BftHf,]■ [C2H5OH] (II) have been determined by single crystal X-ray ana lysis: I is triclinic, space group PI with a = 10.264(2), b = 13.804(2) and c = 20.242(2) A, a = 97.857(10)°, ß = 92.734(11)° and 7 = 103.024(13)°; II is monoclinic, space group P2iIn with a = 12.742(2), b = 7.532(2) and c = 26.887(3) Ä, ß = 95.765(10)°. The 11B NMR spectrum of this compound reveals the feature of monosubstituted octahedral B6 cages. The l3C NMR spectrum exhibits a triplet at 16.20 ppm with '7(C,H) = 120.4 Hz. In the 'H NMR spectrum a singulet at 0.72 ppm of the CH2-groups and two singulets at 1.72 and -4.95 ppm of the BH fragments are observed. The IR and Raman spectra exhibit strong CH stretching bands between 2908 and 2789 cm-1, BH stretching bands between 2463 and 2396 cm-1, and the BC stretching vibration at 1144 in the IR and at 1150 cm" 1 in the Raman spectrum. | | | |
Reference
| Z. Naturforsch. 51b, 363—369 (1996); eingegangen am 3. August 1995 | | | |
Published
| 1996 | | | |
Keywords
| ), Crystal Structure, 'H NMR Spectra, Vibrational Spectra, l3C NMR Spectra, "B NMR Spectra | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0363.pdf | | | | Identifier
| ZNB-1996-51b-0363 | | | | Volume
| 51 | |
| 103 | Author
| G. Erhard, H. Enesa, A. Nton Rieker, M. Arkus, N. Eum Ayerb, W. Olfgang Hiller | Requires cookie* | | | Title
| ,4-Addition of Lithium Organyls to /?ara-Quinols / Structure Determination of 2,6-Di-te/t-butyl-4-hydroxy-4,5-diphenyIcyclohex-2-en-l-one | | | | Abstract
| Addition of lithium organyls to sterically hindered para-quinols leads to 1,2-or 1,4-adducts. The 1,4-addition prevails, if the 4-substituents in the quinol and the organic group in the lithium organyl are large. Four 1,4-addition products (2-cyclohex-2-en-l-ones) are synthesized and their structures investigated by NMR spectroscopy. The aryl groups at C-4 and C-5 acquire equatorial positions, the alkyl group at C-6 is bisectional. These results are confirmed by X-ray analysis of 2,6-di-terr-butyl-4-hydroxy-4,5-diphenylcyclohex-2-en-1 -one, revealing a twist boat conformation of the cyclohexene ring. | | | |
Reference
| Z. Naturforsch. 51b, 381—387 (1996); received August 11 1995 | | | |
Published
| 1996 | | | |
Keywords
| Crystal Structure, Quinol, 1, 4-Addition, Lithium Organyl, Cyclohex-2-en-l-ones | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0381.pdf | | | | Identifier
| ZNB-1996-51b-0381 | | | | Volume
| 51 | |
| 105 | Author
| Rolf Minkwitz, Jens Jakob, Andreas Kornath, Hans Preut | Requires cookie* | | | Title
| Uber die Darstellung, spektroskopische Charakterisierung und Kristallstruktur von Trifluormethylazosulfbn-N,N-dimethylamid (CH3)2N S (0)2NNCF3 On the Preparation, Spectroscopic Characterization and Crystal Structure of Trifluoromethylazosulfon-N,N-dimethylamid (C H 3)2N S (0 )2NNCF3 | | | | Abstract
| The reaction of Trifluoronitrosomethan with (CH3)2NS(0)2N H 2 in T H F and Na2C 0 3 as | | | |
Reference
| Z. Naturforsch. 51b, 557—562 (1996); eingegangen am 10. O ktober 1995 | | | |
Published
| 1996 | | | |
Keywords
| Trifluormethylazosulfon-N, N-dimethylamid, Vibrational Spectra, NM R Spectra, Mass Spectra, Crystal Structure | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0557.pdf | | | | Identifier
| ZNB-1996-51b-0557 | | | | Volume
| 51 | |
| 106 | Author
| Ralf Czekalla, Wolfgang Jeitschko, Rolf-Dieter Hoffmann, Helmut Rabeneck | Requires cookie* | | | Title
| Preparation, Crystal Structure, and Properties of the Lanthanoid Carbides Ln4C7 with Ln = Ho, Er, Tm, and Lu | | | | Abstract
| The isotypic carbides Ln4C7 (Ln = Ho, Er, Tm, Lu) were prepared by arc-melting of the elemental components, followed by annealing at 1300 °C. The positions of the metal and of some carbon atoms of the monoclinic crystal structure of LU4C7 were determined from X-ray powder data, and the last carbon positions were found and refined from neutron powder diffraction data: P2,/c, a = 360.4(1), b = 1351.4(3), c = 629.0(2) pm, ß = 104.97(2)°, Z = 2, R = 0.026 for 429 structure factors and 15 positional parameters. The structure contains isolated carbon atoms with octahedral lutetium coordination and linear Cvunits, with C-C bond lengths of 132(1) and 135(1) pm. This carbide may therefore be considered as derived from methane and propadiene. The hydrolysis of LU4C7 with distilled water yields mainly methane and propine, while the hydrolyses of the corresponding holmium and erbium carbides resulted in relatively large amounts of saturated and unsaturated C2-hydrocarbons in addition to the expected products methane and propine. The structure comprises two-dimensionally infinite NaCl-type building elements, which are separated by the C3-units. It may be described as a stacking variant of a previously reported structure of H04C7, now designated as the a-modification. The Lu4C7-type /^-modification was obtained at higher temperatures. Its structure was refined by the Rietveld method from X-ray powder data to a residual R = 0.037 for 320 F values and 15 positional parameters. Lu4C7 is Pauli paramagnetic; /3-H04C7 and Er4C7 show Curie-Weiss behavior with magnetic ordering temperatures of less than 20 K. | | | |
Reference
| Z. Naturforsch. 51b, 646—654 (1996); received August 28 1995 | | | |
Published
| 1996 | | | |
Keywords
| Binary Lanthanoid Carbides, Magnetic Properties, Hydrolyses of Carbides, Crystal Structure | | | |
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| default:Reihe_B/51/ZNB-1996-51b-0646.pdf | | | | Identifier
| ZNB-1996-51b-0646 | | | | Volume
| 51 | |
| 107 | Author
| Ferdinand Belaj | Requires cookie* | | | Title
| Struktur von C2C16N4P2, dem R eaktionsprodukt von D icyandiam id mit PC15 Structure of C 2C16N4P2, the Reaction Product of Dicyandiamide with PC15 | | | | Abstract
| The reaction product of dicyanodiamide with PC15 (1:2) is 2,2,4-trichloro-2,2-dihydro-6-trichlorophosphazeno-1.3,5,2A5-triazaphosphorine and not 2.4,6-trichloro-2,2-dihydro-2-trichlorophosphazeno-l,3,5,2A5-triazaphosphorine as reported in the literature. This is con firmed by an X-ray structure determination at 90K: Space group P 2,/c, a = 17.258(5), b = 9.664(3), c = 15.070(4) Ä, ß = 114.05(2)°, Z = 8, R = 3.99%. Both molecules of the asymmetric unit show about the same conformation with approximate C s-m -symmetry as was also obtai ned by semi-empirical MNDO calculations. The thermal motion analysis establishes that the molecules cannot be described as 'rigid bodies', and that the easy deformability of the exocyclic C-N-P angles allows the 'rigid' NPC13 tetrahedra to perform almost isotropic librations. | | | |
Reference
| Z. Naturforsch. 51b, 1428—1432 (1996); eingegangen am 20. Februar 1996 | | | |
Published
| 1996 | | | |
Keywords
| 2, 24-Trichloro-2, 2-dihydro-6-trichlorophosphazeno-l, 3, 5, 2A5-triazaphosphorine Phosphaze ne, Crystal Structure, Thermal Motion Analysis | | | |
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| default:Reihe_B/51/ZNB-1996-51b-1428.pdf | | | | Identifier
| ZNB-1996-51b-1428 | | | | Volume
| 51 | |
|
