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1996[X]
101Author    ]. 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 
102Author    Hristoph Linke, M. Artin, JansenRequires cookie*
 Title     
 Abstract    Ag8Ge3O 10 was obtained from a mixture of the binary oxides by solid state reaction in the presence of a small amount of water which is acting as an accelerator. Conditions applied were T = 500 °C and p (0 2) = 1,2 kbar. According to an X-ray crystal structure analysis the title compound contains four crystallographically independent trigermanate [Ge3O 10]8-ions per unit cell (Pc, a = 12.1549(11), b = 10.7375(14), c = 18.5169(20) Ä, ß = 92.326(10)°, 13448 independent reflections, R 1 = 6 ,1 %, wR2 = 13,0%, Z = 8). Thermal decomposition, as recorded by DTA and temperature dependent Guinier photographs, occurs at 520 °C. Ag8Ge3O ,0 is diamagnetic with a molar susceptibility of -330-10" cm3 mol" 1. Darstellung, Kristallstruktur und physikalische Eigenschaften von Oktasilbertrigermanat, Ag8Ge3O10 
  Reference    Z. Naturforsch. 51b, 1591—1597 (1996); eingegangen am 18. April 1996 
  Published    1996 
  Keywords    Octasilver Trigermanate, High Oxygen Pressure Synthesis, Crystal Structure, Physical Properties 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1591.pdf 
 Identifier    ZNB-1996-51b-1591 
 Volume    51 
103Author    M. Athias, O. Sengea, G. Elii, V. P. Ono, M. Arevb, Tim Othy, P. Forsythc, KevinM. Smith0Requires cookie*
 Title    Synthesis, Solution, Molecular and Crystal Structure of Bis[5-(coproporphyrinato-I tetraethylester)nickel(II)]l,2-ethane  
 Abstract    Vilsmeier formylation of the oporphyrin-I tetraethyl ester Ni-complex (III) followed by reduction of the intermediary imine salt (IV) with N aBH4 gave the o-dimethylaminomethyl-coproporphyrin-I Ni-complex (V). Heating the latter in methyl iodide gave 65% of the eth­ ane-bis-porphyrin (I), which has been characterized by NMR-spectroscopy and a molecular and crystal structure investigation. The crystal structure shows an extended structure of the bisporphyrin with a parallel arrangem ent of the porphyrin subunits. Crystal data: I -C90H 106N8Ni2O 16. Triclinic, a = 12.319(3) Ä. b = 13.297(3) A, c = 14.444(3) A, a = 105.56(2)°, ß = 100.82(2)°, y = 112.98(2)°, V = 1981.0(7) A 3, Cu Ka radiation, A = 1.54178 A, space group P I, Z = 1, R = 0.07. 
  Reference    Z. Naturforsch. 51b, 1644—1648 (1996); received April 23 1996 
  Published    1996 
  Keywords    Coproporphyrin-I, Nickel Complex, Vilsmeier Formylation, Ethane-bis-porphyrin Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1644.pdf 
 Identifier    ZNB-1996-51b-1644 
 Volume    51 
104Author    Rolf Minkwitz, Ulrike Lohmann, Hans PreutRequires cookie*
 Title    Primäre und sekundäre Ethyl-und /-Propylsulfoniumsalze sowie Kristallstruktur von /-C3H7SH2+SbF6 [1] Prim ary and Secondary Ethyl and /-Propyl Sulfonium Salts and Crystal Structure of /-C3H 7SH2+SbF6-[1]  
 Abstract    The synthesis of salts of the type R"SH3_"+MF6~ (R = C2H 5, i-C3H 7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/M F5 is reported. The salts have been characterized by vibrational and NM R spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H 7SH 2+SbF6" crystallizes in the monoclinic space group P2i/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, ß = 82.63(6) °, with two formula units per unit cell. 
  Reference    Z. Naturforsch. 51b, 277 (1996); eingegangen am 6. Juli 1995 
  Published    1996 
  Keywords    Primary and Secondary Sulfonium Salts, Vibrational Spectra, NM R Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0277.pdf 
 Identifier    ZNB-1996-51b-0277 
 Volume    51 
105Author    H. Einer, HomborgRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0325.pdf 
 Identifier    ZNB-1996-51b-0325 
 Volume    51 
106Author    Hiromitsu Terao, Tsutomu Okuda, Sachiyo Uyama, Hisao Negita, Shi-Qi Dou, Hartmut Fuess, Alarich WeissRequires cookie*
 Title    Crystal Structure Refinement and Single Crystal 81 Br Zeeman NQR Study of KHgBr 3 H 2 0  
 Abstract    Three 81 Br NQR resonance lines of KHgBr 3 H 2 0 were detected between 77 K and room temperature. From the Zeeman effect measurement on a single crystal the nuclear quadrupole coupling constants (e 2 qQ/h) and the asymmetry parameters (r/) were obtained, which are 228.42 MHz and 0.005, 226.24 MHz and 0.005, and 108.76 MHz and 0.465 for e'qQIh and rj at 295 K, respectively. Large deviations of the observed directions of electric field gradient tensors from the directions expected from previous X-ray results have been found. With the present X-ray redetermination, 1 Br NQR and structure are in good agreement. The structure and bonding in the compound are discussed. 
  Reference    Z. Naturforsch. 51a, 1197—1202 (1996); received June 14 1996 
  Published    1996 
  Keywords    KHgBr v H 2 0, X-Ray analysis, NQR, Crystal structure, Chemical bonding 
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 TEI-XML for    default:Reihe_A/51/ZNA-1996-51a-1197.pdf 
 Identifier    ZNA-1996-51a-1197 
 Volume    51 
107Author    Rolf Minkwitz, Ulrike Lohmann, Hans PreutRequires cookie*
 Title    Methansulfinylchlorid-Lewissäure  
 Abstract    Addukte CH3S(Cl)OMF5 (M = As, Sb) und Kristallstruktur von CH3S(Cl)OSbCl5 [1] Methanesulfinylchloride Lewis Acid Adducts CH3S(Cl)OMF5 (M = As, Sb) and Crystal Structure of CH3S(Cl)OSbCl5 [1] CH 3S(0)C1 reacts in HF as solvent with MF5 (M = As, Sb) to give products CH 3S(Cl)OMF5 (M = As, Sb). The new compounds are stable below 253 K and were charac­ terized by Raman and N M R spectroscopy. In addition, the crystal structure of C H 3S(Cl)OSbCl5 has been determinated. The complex crystallizes in the monoclinic space group P2x !n with a = 644.3(5), b = 1905.9(14), c = 900.0(7) pm, ß = 99.27(6)° with four formula units per unit cell. 
  Reference    Z. Naturforsch. 51b, 133—138 (1996); eingegangen am 6. Juni 1995 
  Published    1996 
  Keywords    Methanesulfinylchloride Lewis Acid Complexes, Preparation, Raman Spectra, N M R Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0133.pdf 
 Identifier    ZNB-1996-51b-0133 
 Volume    51 
108Author    Hans Bock, Sabine Nick, Wolfgang Seitz, Christian Näther, JanW. BatsRequires cookie*
 Title    Structures of Charge-Perturbed or Sterically Overcrowed Molecules, 80 [1 -3] Structural Changes of /?-Benzoquinone by Donor and Acceptor Substituents  
  Reference    Z. Naturforsch. 51b, 153—171 (1996); eingegangen am 29. Mai 1995 
  Published    1996 
  Keywords    Crystal Structure, Oxo-and Alkylamino-Substituted p-Benzoquinone Derivatives, Substituent Effects, Cyanine Distortion, AM 1 Calculations 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0153.pdf 
 Identifier    ZNB-1996-51b-0153 
 Volume    51 
109Author    W. Lübbe, W. PreetzRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0363.pdf 
 Identifier    ZNB-1996-51b-0363 
 Volume    51 
110Author    G. Erhard, H. Enesa, A. Nton Rieker, M. Arkus, N. Eum Ayerb, W. Olfgang HillerRequires 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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 Identifier    ZNB-1996-51b-0381 
 Volume    51 
111Author    W. Preetz, B. SteuerRequires cookie*
 Title    Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der 10B-und n B-Isotopomeren von [B2(NCS)6]2_ sowie Kristallstruktur von (Ph3P=N=PPh3)2[B2(NCS)6]  
 Abstract    By reaction of [B6H 6]2_ with a solution of (SCN)2 in dichloromethane in the presence of solid KOH the hexaisothiocyanatodiborate anion [B2(NCS)6]2~ is formed and can be isolated by fractionated crystallization. The crystal structure of (PNP)2[B2(NCS)6] has been determ i­ 
  Reference    Z. Naturforsch. 51b, 551—556 (1996); eingegangen am 11. August 1995 
  Published    1996 
  Keywords    H exaisothiocyanatodiborate(2-), Crystal Structure, Vibrational Spectra, Isotopomers, Normal Coordinate Analysis 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0551.pdf 
 Identifier    ZNB-1996-51b-0551 
 Volume    51 
112Author    Rolf Minkwitz, Jens Jakob, Andreas Kornath, Hans PreutRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0557.pdf 
 Identifier    ZNB-1996-51b-0557 
 Volume    51 
113Author    Ralf Czekalla, Wolfgang Jeitschko, Rolf-Dieter Hoffmann, Helmut RabeneckRequires 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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0646.pdf 
 Identifier    ZNB-1996-51b-0646 
 Volume    51 
114Author    H. Bock, C. Arad, C. Näther, I. G. Öbel, A. John, R. BaurRequires cookie*
 Title    Elektronentransfer und Kontaktionen-Bildung, 45 [1, 2] Strukturänderungen bei der Einelektronen-Reduktion von Tetraphenyl- butatrien zum Radikalanion und bei der Zweifach-Deprotonierung von Tetraphenyl-butin-2 zum Tetraphenylbutatrien-Dianion Electron Transfer and Contact Ion Pair Form ation, 45 [1 ,2 ] Structural Changes on Single Electron R eduction of Tetraphenylbutatriene to its Radical A nion and on Twofold D eprotonation of Tetraphenylbutyne-2 to the Tetraphenylbutatriene D ianion  
 Abstract    Tetraphenylbutatriene is reduced under aprotic conditions to its ESR/ENDOR-spectro-scopically characterized radical anion and to its dianion, with both electron transfers quasi-reversible according to cyclovoltammetric measurements. The alkali cation salts, the red con­ tact ion pair [(H ^C ^C j K N a^H iC O C H iC H iO C H ^d and the dark violet contact ion triple [(H3C6)4C4" ' KLi^H ^CO CH iCIU O CH O ?^ can be prepared by single electron reduction at a sodium metal mirror or by twofold de-protonation of l,l,4,4-tetraphenylbutyne-2 using lithium-/;-butyl. Their single crystal structures as well as that of the parent acetylene have been determined at low temperatures. The essential structural changes observed are the twisting of both molecular halves (H5C6)2CC relative to each other with increasing negative charge. The simultaneously resulting bond alternancy >C = C = C = C< — >Ce -C = C -C < within the cumulene chain is discussed based on MNDO calculations for the structures determined. Ausgangspunkt: Die Strukturen von K um ulenen 
  Reference    Z. Naturforsch. 51b, 1381—1390 (1996); eingegangen am 15. November 1995 
  Published    1996 
  Keywords    Tetraphenylbutatriene Radical Anion and Dianion Salts, Cyclovoltammetry, ESR/ENDOR Spectra, Single Crystal Structures 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1381.pdf 
 Identifier    ZNB-1996-51b-1381 
 Volume    51 
115Author    Ferdinand BelajRequires 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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 Identifier    ZNB-1996-51b-1428 
 Volume    51 
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