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1984 (324)
41Author    Mario Cannas, Giaime Marongiu, HeimoJ. Keller, Barbara Müller, Reinhold MartinRequires cookie*
 Title    Structure of the Linear-Chain Mixed Valence Compound Bis(l,3-diaminopropane)platinum(II)bis(l,3-diaminopropane)- diiodoplatinum(IV)tetraperchlorate  
 Abstract    The title compound CpH49Cl4LN80 16Pt-,, Mr 1314.1, is monoclinic P 2, (from structural analy­ sis), a = 8.74(1), b = 11.36(1), c = 8.63(1), ß = 107.6(5), V = 817 Ä 3, Z = 1, D m (flotation) = 2.65 g cm-3, D c = 2.66 g cm-3, MoKa A = 0.71069, /u = 110.7 cm-1, R = 0.063 for 1068 observed reflections. Rotation photographs show diffuse patterns corresponding to odd values of k together with weak Bragg reflections. Refinement of diffractometer data was carried out in space groups Pm, P2,/m and P2,; both refinement in Pm and P2, give satisfactory agreement and lead to very similar crystal structures. 
  Reference    Z. Naturforsch. 39b, 197 (1984); eingegangen am 5. September 1983 
  Published    1984 
  Keywords    Linear Chain, Mixed-Valence Platinum(II, IV) Compound 
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 Identifier    ZNB-1984-39b-0197 
 Volume    39 
42Author    M. Witzei, D. BabelRequires cookie*
 Title    Die Kristallstruktur des elpasolith-verwandten Cyanokomplexes [N(CH3)4]2NaFe(CN)6 * H20 The Crystal Structure of the Elpasolite-Related Cyano Complex [N(CH3)4]2NaFe(CN)6 * H20  
 Abstract    The compound [N(CH3)4]2NaFe(CN)6 • H20 crystallizes in the orthorhombic space group Pnma, Z = 4, a — 1863.9(2), b = 861.7(1), c — 1317.2(2) pm. The X-ray single crystal structure determination (2515 reflections, R — 0.04) revealed an elpasolite-related framework of slightly deformed Fe(CN)63_ octahedra, the mean distances in which are Fe —C = 194.0 and C—N = 113.9 pm. The strongly distorted octahedral N6 cavities formed by six Fe(CN)63_ units are occupied by monohydrated sodium ions, exhibiting a very short distance N a—O = 221.8(3) pm. By approach to one of the octahedral faces within their N6 environment the sodium ions obtain a distorted tetrahedral NaON3 coordination, N a—N = 2 x 238.0(3) and 241.3(3) pm. One of the compound's two tetramethylammonium ions, which are centered at mirror planes, is orientation-ally disordered. The reason for this is discussed. 
  Reference    Z. Naturforsch. 39b, 201 (1984); eingegangen am 21. Juli/19. Oktober 1983 
  Published    1984 
  Keywords    Crystal Structure, Elpasolite, Hexacyanoferrate(III), Monohydrated Sodium Ion 
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 Identifier    ZNB-1984-39b-0201 
 Volume    39 
43Author    Karl Dimroth, Rüdiger Thamm, Hans KaletschRequires cookie*
 Title    öjr-Tricarbonyl-Komplexe von Pyridin-Derivaten, Synthesen und Reaktionen 6 ;r-Tricarbonyl-Chromium Complexes of Pyridine Derivatives, Syntheses and Reactions  
 Abstract    New ö^-tricarbonylchromiumpyrnftne complexes 5c and 5d could be synthesized from 2,6-di-r-butyl-and 2,4,6-tri-f-butylpyridines (3c and 3d) with chromium hexacarbonyl. They are charac­ 
  Reference    Z. Naturforsch. 39b, 207 (1984); eingegangen am 14. September 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0207 
 Volume    39 
44Author    RolandE. Schmidt, Werner MassaRequires cookie*
 Title    Die Kristallstruktur von Tricarbonyl(2.6-di-rm-butyl-pyridin)chrom(0) bei 200 K Crystal Structure of Tricarbonyl(2,6-dwerr-butyl-pyridine)chromium(0) at 200 K  
 Abstract    Based on single crystal X-ray diffraction data the crystal structure of tricarbonyl(2,6-dwm-butyl-pyridine)chromium(O) has been determined at 200 K: space group P 2,/n, Z = 4, lattice constants a = 680.6(5), b — 1383.3(10), c = 1763.0(16) pm, ß = 96.53(8)°, refinement to R" — 0.048 for 1672 independent reflections with F0 > 2 a. The chromium atom is ^ ^ -b o n d ed to the essentially planar pyridine ring (Cr—C: 219—222 pm, Cr—N: 221 pm). The CO ligands show "eclipsed" orientation with respect to the 2, 4 and 6 position of the pyridine ring. Two CO groups fit into the gaps formed by two methyl groups of the tert-butyl substituents in 2 and 6 position, respectively. The results are discussed in context with related arene and A3-phosphorine com­ plexes. 
  Reference    Z. Naturforsch. 39b, 213 (1984); eingegangen am 14. September 1983 
  Published    1984 
  Keywords    Pyridine Complex, Tricarbonyl Chromium Complex, Crystal Structure 
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 Identifier    ZNB-1984-39b-0213 
 Volume    39 
45Author    Heinz-Peter Schuchmann, Clemens Von SonntagRequires cookie*
 Title    Methylperoxyl Radicals: A Study of the y-Radiolysis of Methane in Oxygenated Aqueous Solutions  
 Abstract    A product study has been made of the y-radiolysis of aqueous methane solutions that also contained nitrous oxide and oxygen. Formaldehyde (G = 2.8), hydrogen peroxide (G = 2.1), methanol (G = 1.5), methylhydroperoxide (G = 0.8), formic acid (G = 0.3), and dimethylper-oxide (G = 0.1) were found. In alkaline solutions (pH 8, 10-3 M phosphate buffer), the formal­ dehyde yield rises to G = 3.2, while the formic acid yield falls to almost zero (G = 0.05). The initial precursor of the carbon-containing products is the methylperoxyl radical. The methyl­ peroxyl radicals decay through a short-lived tetroxide along various pathways. The most promi­ nent one leads to formaldehyde, methanol and oxygen. Methoxyl radicals (and oxygen) are also formed and, after rearrangement into hydroxymethyl radicals and their conversion into hy-droxymethylperoxyl radicals, eventually yield formic acid and probably further formaldehyde. A route to formaldehyd and hydrogen peroxide is also envisaged. Methylhydroperoxide is formed in the reaction of methylperoxyl radicals with H 0 2 / 0 27 radicals (from radiolytic H atoms and the unimolecular decay of the hydroxymethylperoxyl radical). 
  Reference    Z. Naturforsch. 39b, 217 (1984); received September 19 1983 
  Published    1984 
  Keywords    Autoxidation, Peroxyl Radicals, Oxyl Radicals, Radical Rearrangements, Radiation Chemistry 
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 Identifier    ZNB-1984-39b-0217 
 Volume    39 
46Author    JohannWalter Buchler, Christine DreherRequires cookie*
 Title    Metallkomplexe mit Tetrapyrrol-Liganden, XXXIII [1] Darstellung von Azidochrom(III)-, Azidomangan(III)-und Azidoeisen(III)-Porphyrinen und deren Photolyse zu terminalen oder verbrückten Nitridometallporphyrinen Metal Complexes with Tetrapyrrole Ligands XXXIII [1] Preparation of Azidochromium(III)-, Azidomanganese(III)-, and Azidoiron(III) Porphyrins and their Photolysis to Terminal or Bridged Nitridometal Porphyrins  
 Abstract    Azidometal(III) porphyrins, e.g. M(TTP)N3 lA a— ICa (M = Cr, Mn, Fe), are transformed 
  Reference    Z. Naturforsch. 39b, 222 (1984); eingegangen am 29. August 1983 
  Published    1984 
  Keywords    Chromium Porphyrins, Manganese Porphyrins, Nitridometal Complexes, Photolysis of Azido Complexes 
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 Identifier    ZNB-1984-39b-0222 
 Volume    39 
47Author    O. Tto, O. Lfb, Onowara Begum2, Hans GeigerbRequires cookie*
 Title    Fluorescence Properties of Hydroxy-and Methoxyflavones and the Effect of Shift Reagents  
 Abstract    The fluorescence spectra o f 42 hydroxy-and m ethoxyflavones in m ethanol solution have been investigated. The follow ing findings are considered to be useful in structure elucidation and identification o f flavonoids: (a) The maxima of the absorption and fluorescence bands give, in m ost cases, a unique combination; (b) flavones exhibit exceptionally large Stok es' shifts (6,800 to 
  Reference    Z. Naturforsch. 39b, 231 (1984); received Septem ber 23 1983 
  Published    1984 
  Keywords    Flavonoids, F luorescence, Structure Elucidation, Shift Reagents 
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 Identifier    ZNB-1984-39b-0231 
 Volume    39 
48Author    O. Tto, S. W. Olfbeis, Eva Fiirlinger3, HemC. Handra Jhab, Fritz ZillikenbRequires cookie*
 Title    The Absorption and Fluorescence of Isoflavones and the Effect of Shift Reagents  
 Abstract    The absorption and fluorescence maxima o f 20 isoflavones have been determ ined in methanol solution and the effect o f addition o f w ater, 50% sulfuric acid, aluminium trichloride, borax, sodium acetate, ammonia and sodium hydroxide has been studied. The following findings may be useful in the structure elucidation o f naturally occurring isoflavones: (a) 5-Hydroxyisoflavones have band I absorption maxima around 335 nm. 6-hydroxyisoflavones betw een 310 and 330 nm, 
  Reference    Z. Naturforsch. 39b, 238 (1984); received Septem ber 23 1983 
  Published    1984 
  Keywords    Isoflavonoids, F luorescence, A bsorption, Shift Reagents 
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 Identifier    ZNB-1984-39b-0238 
 Volume    39 
49Author    H. Artm, Ut LaatschRequires cookie*
 Title    Dimeric N aphthoquinones, X* A Convenient Synthesis of Desapogossypolone Tetraethyl E ther  
 Abstract    Professor H. B rockm ann zu m 80. Geburtstag gew idm et Dimeric N aphthoquinones, O xidative C oupling, B enz[f]indazolequinones D esapogossypolone tetraethyl (2 b), a degradation product o f gossypol (1), was obtained in a simple way by oxidative coupling o f 6,7-diethoxy-4-m ethoxy-l-naphthol (7c) and C-methylation with diazom ethane. 
  Reference    Z. Naturforsch. 39b, 244 (1984); eingegangen am 11. August 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0244 
 Volume    39 
50Author    G. Lutz, Ro Tjah, V. Olker, B. K. Oppenhagenab, Ludger Ernst3, G. Bf, —. G. Esellschaft Für, B. Iotechnologische Forschung, M. Ascheroder, W. EgRequires cookie*
 Title    Fast Atom Bombardment Mass Spectrometry of the Vitamin B12 Analogues Hydrogenobalamin and Cupribalamin  
 Abstract    H ydrogenobalam in, Cupribalamin, Mass Spectrometry H ydrogenobalam in (m etal-free vitamin B 12) and cupribalamin are characterized by their fast atom bom bardm ent (F A B) mass spectra which show molecular ion and characteristic fragm ent ion peaks. T hese spectra and the high-resolution FAB mass spectrum o f cobalamin (vitam in B 12) show that the (M + H)+-C N -5 9 peak for the latter is due to loss of acetam ide and not o f the central cobalt atom . In the F A B mass spectrum of cupribalamin metal clusters are observed. 
  Reference    Z. Naturforsch. 39b, 248 (1984); received July 26 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0248 
 Volume    39 
51Author    Delbert BacherRequires cookie*
 Title    Biosynthesis of Riboflavin Preparation of Phosphorylated Pyrimidine Intermediates  
 Abstract    Riboflavin, Biosynthesis, 2,5-D iam ino-6-ribitylam ino-4(3H)-pyrim idinedione 5'-Phosphate, 5-A m ino-6-ribitylam ino-2,4(l H ,3H)-pyrim idinedione 5'-Phosphate, Pyrimidine D eam inase 
  Reference    Z. Naturforsch. 39b, 252 (1984); received Septem ber 1 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0252 
 Volume    39 
52Author    Tetraphenylarsonium, Edgar Bilger, Jürgen Pebler, R. Ainer, W. Eber, Kurt DehnickeRequires cookie*
 Title    N O T IZ E N  
 Abstract    -tetraoxoosinat(VII), A sP h4[O sÖ 4] Tetraphenylarsonium Tetraoxoosm ate(V II), AsPh4[ 0 s 0 4] Tetraphenylarsonium T etraoxoosm ate(V II), Syn­ thesis, IR Spectra, M agnetic M om ent, Cyclic Volt-ammetry A sP h4[ 0 s 0 4] is prepared by reaction of 0 s 0 4 with A sP h4I in C H :C12 solution. According to the IR spectrum , the [O sO 4]0 ion adopts a distorted tet­ rahedral structure. The reciprocal magnetic suscep­ tibility displays linear temperature dependence in 
  Reference    Z. Naturforsch. 39b, 259 (1984); eingegangen am 7. O ktober 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0259_n 
 Volume    39 
53Author    RainerW. Eber, Kurt DehnickeRequires cookie*
 Title    Nitrosyl-und Thionitrosylkomplexe des Osmiums: [Os(NO)C15]9 und [Os(NS)CI5]G Nitrosyl-and Thionitrosyl Complexes of Osmium: [O s(N O )Cl5]e and [Os(NS)C15]q  
 Abstract    Osmium pentachloride reacts with NO forming the com plex N O [O s(N O)C l5], which when treated with (PPh3M e)C l yields PPh3M e[O s(N O)C l5] and nitrosyl chloride. The thionitrosyl com plex A sP h 4[O s(N S)C l5] is prepared by the reaction of 
  Reference    Z. Naturforsch. 39b, 262 (1984); eingegangen am 7. O ktober 1983 
  Published    1984 
  Keywords    Peptachloronitrosyl-osm ate, Pentachlorothionitrosyl-osm ate, Preparation, IR Spectra 
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 Identifier    ZNB-1984-39b-0262_n 
 Volume    39 
54Author    O. Tto Schneider, Michael HanackRequires cookie*
 Title    Phthalocyaninatoeisen-Cyanid- Verbindungen: Synthese und elektrische Leitfähigkeiten Cyanide Containing Phthalocyaninatoiron Compounds: Synthesis and Electrical Conductivities  
 Abstract    (w-Cyano)phthalocyaninatoiron(II), -iron(III), Thermal Analysis, Electrical Conductivity The preparation o f cyanide containing phthalocy-aninatoiron(II) or -iron(III) derivatives either with terminal or bridging cyanide is described. With help o f the C = N valence frequency (IR) and the m agnet­ ism of the com pounds the oxidation state o f the iron is determined. Therm oanalytical and electrical con­ ductivity data are reported. 
  Reference    Z. Naturforsch. 39b, 265 (1984); eingegangen am 10. O ktober 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0265_n 
 Volume    39 
55Author    Franz Dirschl, Heinrich NöthRequires cookie*
 Title    Kristall-und Molekülstrukturen von zwei fraws-1.2.4.5-Tetraza-3.6-diphospha-cyclohexan-3.6-disulfiden Crystal and M olecular Structures of Two trans-l ,2,4,5-Tetraza-3,6-diphospha-cyclohexane-3,6-disulfides  
 Abstract    X -R ay, frans-H exam ethyl-l,2,4,5-tetraza-3,6-diphospha-cyclohexane-3,6-disulfide, rran.s-l,2,4,5-Tetram ethyl-3,6-diphenyl-l,2,4,5-tetraza-3,6-diphospha-cyclohexane-3,6-disulfide 
  Reference    Z. Naturforsch. 39b, 269 (1984); eingegangen am 29. Juli 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0269 
 Volume    39 
56Author    Marianne Bäudler, V. Olker, A. RndtRequires cookie*
 Title    Contributions to the Chem istry of Phosphorus, 135 [1] Synthesis and Structures of Novel Polycyclic Organophosphanes PnR m (m < n)  
 Abstract    T ricyclo[4.3.0.03 7]nonaphosphanes, Tricyclo[5.2.1.02'6]-and T etracyclö[5.2.1.02-6.03 8]decaphosphanes, Tetracyclo[6.2.1.02'6.051()]undecaphosphanes, Penta-cyclo[6.4.0.0 2-6.0512.0711]dodecaphosphanes, Pentacyclo[7.4.0.02'6.05 13.08,12]tridecaphosphanes 
  Reference    Z. Naturforsch. 39b, 275—283 (1984); eingegangen am 11. O ktober 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0275 
 Volume    39 
57Author    Heinz-W Erner, Hennig, Peter Sartori, Ulrich SteinbrechtRequires cookie*
 Title    Carboxydiphenyl Phosphane Sulfides  
 Abstract    Carboxydiphenyl Phosphane Sulfides, Thermal Stability Carboxydiphenyl phosphane sulfides (Cf,H5)^ P (S)(0 C (0)R) (2) (R = CFL 2a, C^Hs 2b. C 17H 3S 2c, (C H 3)3C 2d. C6H 5 2e) were prepared by reacting silver salts of carboxylic acids A g 0 C (0) R with (C 6H 5)2P(S)C1 (Schem e 1) or by treating carboxylic acids with (C6H 5)2P(S)C1 in the presence of triethyl amine (Schem e 2) and spectroscopically characterized. Thermal stability and stability against hydrolysis of the m ixed anhydrides is unusually high. 
  Reference    Z. Naturforsch. 39b, 284 (1984); eingegangen am 7. N ovem ber 1983 
  Published    1984 
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 Identifier    ZNB-1984-39b-0284 
 Volume    39 
58Author    Dietrich Mootz, Wolfgang PollRequires cookie*
 Title    Fluoride und Fluorosäuren, VI Verbindungsbildung und Kristallstrukturen im System Ammoniak—Fluorwasserstoff [ 1 , 2 ] Fluorides and Fluoro Acids, VI Com pound Form ation and Crystal Structures in the System A m m onia-H ydrogen Fluoride  
 Abstract    The melting diagram of the quasi-binary system NH3— HF between the limits NH4HF: and HF was redetermined. The compounds NH 3 • 4H F. NH3 • 5HF and NH3 ■ 8HF with melting points of 26. —14 (dec.) and —95 °C (dec.), respectively, were established as the stable phases. Their crystal structures were determined as those of ammonium hydrogen fluorides NH4[F(HF)3], NH4[F(HF)4] and NH4[HF:(H F)3] • 3HF with extended N -H --F and F -H -F hydrogen bonding. 
  Reference    Z. Naturforsch. 39b, 290—297 (1984); eingegangen am 15. September 1983 
  Published    1984 
  Keywords    System NH3 — HF, Melting Diagram Crystal Structure, Hydrogen Bonding 
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 Identifier    ZNB-1984-39b-0290 
 Volume    39 
59Author    Dietrich Mootz, D. Agm Ar BoenigkRequires cookie*
 Title    Fluoride und Fluorosäuren, VII [1] Kristallstrukturen von Säurehydraten und Oxoniumsalzen, XXII [2] Hydratbildung der Trifluoressigsäure sowie Strukturen eines Monohydrats und eines Tetrahydrats [3] Fluorides and Fluoro Acids, VII [1] Crystal Structures of Acid H ydrates and Oxonium Salts, XXII [2] H ydrate Form ation of Trifluoroacetic Acid and Structures of a M onohydrate and a Tetrahydrate [3]  
 Abstract    The liquidus and solidus lines of the quasi binary system CF3C O O H —H20 were determined by low temperature difference thermal analysis and the resulting phase relations controlled by X-ray powder diffraction. Formation of a monohydrate and a tetrahydrate, melting congruently at —43 and —16 °C, respectively, is confirmed. In addition a metastable form of the monohydrate and a low temperature form of the tetrahydrate, stable below —47 °C, are indicated. The crystal struc­ tures of the stable high temperature forms were determined. From these the monohydrate (tetra­ gonal, space group I42d, Z = 16) is a true acid hydrate, C F ,C 0 0 H H 20 . and the tetrahydrate (triclinic, P I, Z -2) a hydrated oxonium salt, (H 50 2) + [H(CF3COO)2]~ • 6 H:0 . 
  Reference    Z. Naturforsch. 39b, 298—3 (1984); eingegangen am 8. November 1983 
  Published    1984 
  Keywords    Trifluoroacetic Acid, Hydrates, Phase Diagram, Crystal Structure, Hydrogen Bonding 
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 Identifier    ZNB-1984-39b-0298 
 Volume    39 
60Author    Rüdiger Kniep, LutzK. Örte, Dietrich MootzRequires cookie*
 Title    Phasenbeziehungen im System Schwefel—Chlor sowie Kristallstrukturen von SC12 und SC14 [1] Phase Relations in the System Sulfur—Chlorine and Crystal Structures of SC12 and SC14  
 Abstract    From new DT A and powder diffraction measurements in the binary system sulfur-chlorine a consistent construction of the melting diagram for the region 50—100 atom-% Cl was possible. It contains sulfur chlorides of the elemental ratios 1:1, 1:2, 1:3, and 1:4 as the stable intermediate phases, which melt at -8 0 °C (congr.), —125 °C (incongr.), —75 °C (incongr.) and — 34 °C (congr.), respectively. SCI is S2C12 as characterized by its crystal structure by R. Kniep, L. Korte 
  Reference    Z. Naturforsch. 39b, 305 (1984); eingegangen am 27. September 1984 
  Published    1984 
  Keywords    Phase Relations, Sulfur Halides, Crystal Structure 
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 Identifier    ZNB-1984-39b-0305 
 Volume    39 
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