| | 101 | Author
| H.-R Schulten | Requires cookie* | | | Title
|  | | | | Abstract
| A combined 13 C nuclear magnetic resonance and field desorption mass spectrometric investigation of algae grown on 13 C02 has shown that the isotopic enrichment of amino acids extracted therefrom is neither uniform nor statistical. The use of these two indepen-dent techniques allows a new, detailed and accurate insight into the label distribution resulting from biosynthesis. The observed deviations from the statistical abundances are systematic. A system for classifying each member of the complex ensemble of isotopic species has been devised, so that the isotopomers may be ordered according to their relative probability of occurrence. | | | |
Reference
| Z. Naturforsch. 36b, 1289—1296 (1981); received May 20 1981 | | | |
Published
| 1981 | | | |
Keywords
| 13 C Enriched Amino Acids, Biosynthesis, Label Distribution, NMR Spectra, Field Desorption Mass Spectrometry | | | |
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| default:Reihe_B/36/ZNB-1981-36b-1289.pdf | | | | Identifier
| ZNB-1981-36b-1289 | | | | Volume
| 36 | |
| 102 | Author
| PeterM. Kaiser®, Reinhard Nesper, Karl-Friedrich Tebbe, Herbert Witzel»- | Requires cookie* | | | Title
| Pyridin-4-on-Nueleosid + : Stabilisierung der Struktur im Kristall und in wäßriger Lösung Pyridine-4-on Nucleoside: Stabilisation of the Structure in the Crystal and in Aqueous Solution | | | | Abstract
| C10H13NO5 • H2O is monoclinic, space group P2i with a = 773.7 pm, b = 814.6 pm, c= 932.6 pm, ß = 109.36° at 143 K, Z = 2. The crystal structure has been refined to R =0.031 with 1340 counter reflections. Features of this nucleoside include an orientation of the base at the glycosidic bond N(l)-C(l') in the anii-range (52.5°), a ribosyl moiety in the C(2')-endo(S) conformation and in contrast to many other nucleosides a trans arrange-ment at C(4')-C(5'). This unusual conformation is stabilized by a distinct H-bonding scheme including the water molecule and the oxygen of the adjacent pyridin-4-on ring system. NMR data indicate on the other side that in solution the conformation of the nucleoside is anti/g + similar to that of other pyrimidine nucleosides. The 5'-OH group replaces the water molecule in the crystal. The preferred anti position of the base cannot be explained by an interaction of H(2,6) of the base with the 5'-OH group or the C(4) oxygen. Both protons which couple with H(3,5) coalesce in a single sharp doublet. Water entropy seems to be the decisive factor for the stabilization of the anti/g+ conformation in aqueous solution. | | | |
Reference
| Z. Naturforsch. 36b, 1632—1639 (1981); eingegangen am 3. Juli 1981 | | | |
Published
| 1981 | | | |
Keywords
| Pyridine-4-on Nucleoside, X-ray, NMR Spectra, Conformational Differences, Water Entropy | | | |
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| default:Reihe_B/36/ZNB-1981-36b-1632.pdf | | | | Identifier
| ZNB-1981-36b-1632 | | | | Volume
| 36 | |
| 106 | Author
| Jochen Ellermann, AlfonsA M Demuth | Requires cookie* | | | Title
| Chemistry of Poly functional Molecules, 75 [1] The Reaction of 5-Bromo-uracil with Sodium Diphenylphosphide | | | | Abstract
| 5-Bromo-uracil (1) reacts with sodium diphenylphosphide or a mixture of sodium diphenylphosphide and sodium amide in liquid ammonia to give sodium 5-bromo-uracilate (5 a). From water 5 a crystallizes with one mole H2O yielding 5b. Treatment of 5 a with D2O yields sodium 5-bromo-N-deutero-uracilate-D20 (1/1) (5 c). With chlorodiphenyl-phosphine 5a forms 1-diphenylphosphino-uracil (2). 5a, b, c show N(l)-N(3)-(H/D)-tauto-merism in concentrated D2O solutions already, but in DMSO or Dö-DMSO only in dilute solutions. All the compounds were characterized by infrared, Raman, X H NMR, UV spectra and conductometry. | | | |
Reference
| Z. Naturforsch. 38b, 1568—1574 (1983); eingegangen am 6. Juni/2. August 1983 | | | |
Published
| 1983 | | | |
Keywords
| Sodium 5-Bromo-uracilates, Deutero Derivatives, Tautomerism, NMR Spectra, UV Spectra, Vibrational Spectra | | | |
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| default:Reihe_B/38/ZNB-1983-38b-1568.pdf | | | | Identifier
| ZNB-1983-38b-1568 | | | | Volume
| 38 | |
| 107 | Author
| Udo Kunze, Andreas Bruns | Requires cookie* | | | Title
| Phosphinsubstituierte Chelatliganden, XII [1] Metallinduzierte E/Z-Isomerisierung an Rheniumcarbonyl-Komplexen mit Phosphinothioformamid-und -thioformimidat-Liganden Phosphine-Substituted Chelate Ligands, XII [1] Metal-Induced E/Z-Isomerisation of Rheniumcarbonyl Complexes with Phosphino- thioformamide and -thioformimidate Ligands | | | | Abstract
| The coordination of tertiary phosphinothioform-amides and the isomeric S-alkyl phosphinothioform-imidates to BrRe(CO) 5 gives the /ac-bromotricar-bonylrhenium complexes la, b and 2a, b with P,S-chelate ligands. Unlike the analogous manganese complexes, the NMR spectra of dissolved lb and 2a, b show a splitting of the N-alkyl ('H, 13 C) and phosphorus signals indicating E/Z isomerisation of the ligands. | | | |
Reference
| (Z. Naturforsch. 40b, 127—128 [1985]; eingegangen am 7. August/5. September 1984) | | | |
Published
| 1985 | | | |
Keywords
| E/Z-Isomerisation, NMR Spectra, Rhenium Complexes, Tertiary Phosphinothioform-amides, S-Alkyl Phosphinothioformimidates | | | |
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| default:Reihe_B/40/ZNB-1985-40b-0127_n.pdf | | | | Identifier
| ZNB-1985-40b-0127_n | | | | Volume
| 40 | |
| 108 | Author
| Dieter Hellwinkel, Peter Ittemann, Siegbert Bohnet | Requires cookie* | | | Title
| Dibenzo | | | | Abstract
| [b,g]heterocin-5,7-dione Dibenzo[b.g]heterocine-5,7-diones | | | |
Reference
| Z. Naturforsch. 40b, 858—859 (1985); eingegangen am 13. Februar 1985 | | | |
Published
| 1985 | | | |
Keywords
| Dibenzo[b, g]heterocine-5, 7-diones, Synthesis, NMR Spectra, Stereochemistry, Ring Inversion | | | |
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| default:Reihe_B/40/ZNB-1985-40b-0858_n.pdf | | | | Identifier
| ZNB-1985-40b-0858_n | | | | Volume
| 40 | |
| 109 | Author
| W. Erner, M. Artin, E. Bner, W. Erner Bertleff | Requires cookie* | | | Title
| CS2, CSSe und CSe2 als Bausteine für ein-und zweikernige Palladium-und Platinkomplexe [1] CS2, CSSe and CSe2 as Building Blocks for Mono-and Binuclear Palladium and Platinum Complexes [1] H elm ut | | | |
Reference
| Z. Naturforsch. 40b, 1351 (1985); eingegangen am 11. Juni 1985 | | | |
Published
| 1985 | | | |
Keywords
| Mononuclear Phosphanepalladium Complexes, NMR Spectra, Binuclear Complexes, Bridging Heteroallenes C EE', Zwitterions PR3CEE' as Ligands | | | |
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| default:Reihe_B/40/ZNB-1985-40b-1351.pdf | | | | Identifier
| ZNB-1985-40b-1351 | | | | Volume
| 40 | |
| 111 | Author
| Udo Kunze, Rolf Tittmann | Requires cookie* | | | Title
| Phosphinsubstituierte Chelatliganden, XXIII [1] Darstellung und NMR-Spektren von Alkyl-arylphosphinothioformamiden, R(Ph)PC(S)NHMe Phosphine-Substituted Chelate Ligands, XXIII [1] Synthesis and NMR Spectra of Alkyl-arylphosphinothioformamides, R(Ph)PC(S)NHMe | | | | Abstract
| A series of alkyl-arylsubstituted N-methyl phosphinothioformamides, R(Ph)PC(S)NHMe (2 a—g), with varying bulkiness of the alkyl rest was synthesized from the racemic secondary phosphines la—g and methyl isothiocyanate. 'H and 13 C NMR spectra of 2a—g reveal signal sets of diastereotopic nuclei due to the asymmetry of the molecule. The chemical shift and coupling constants were confirmed by simulation in case of 2b, c. The vicinal 31 P— 13 C cou-plings of the menthyl and neomenthyl compounds 2f, g show an "anti-Karplus" behaviour CJ(gauche) > ? J(trans)) and allow the conformational assignment of the alicyclic group. The 31 P chemical shifts of 2a—d give a linear correlation with the cone angle of the alkyl substituents quoted from literature. | | | |
Reference
| (Z. Naturforsch. 42b, 77—83 [1987]; eingegangen am 8. August 1986) | | | |
Published
| 1987 | | | |
Keywords
| Alkyl-arylphosphinothioformamides, Menthyl and Neomenthyl Derivatives, NMR Spectra, Conformational Analysis, Substituent Influence | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0077.pdf | | | | Identifier
| ZNB-1987-42b-0077 | | | | Volume
| 42 | |
| 112 | Author
| Franjo Gol, Gerd Hasselkuß, PeterC. Knüppel, Othmar Stelzer | Requires cookie* | | | Title
| Lineare Oligophosphaalkane, XX [1] Alkalimetall-und Trimethylsilylderivate PH-funktioneller Methylenbisphosphane Linear Oligophosphaalkanes, XX [1] Alkali Metal and Trimethylsilyl Derivatives of PH-Functional Methylenebisphosphanes | | | | Abstract
| The synthesis of the trimethylsilyl derivatives of the PH-functional methylenebisphosphanes, R 2 ^"(Me 3 Si)"P—CH 2 —PR(SiMe 3) (R = Me. /Pr. tBu. Ph. 2.4.6-Me 3 C (,H 2 ; n = 0. 1) is reported. In the Li-phosphides R 2 _"Li"P — CH 2 — PUR used as reactive intermediates, a monomer-oligomer association equilibrium causes a rapid Li-exchange as indicated by the solvent and temperature dependent ^PI'H} and 7 Li NMR spectrum of (/Pr) 2 P-CH 2 -P(/Pr)Li in various solvents (Et : 0. THF and MTHF) in the temperature range from 30 to -110 °C. For the syntheses of the Me-and Ph-substituted PH-functional methylenebisphosphanes R 2 P-CH 2 -PRH and RHP-CH 2 -PRH (R = Me, Ph) the chlorophosphane CKP —CH 2 —PC1 2 is used as a starting material. Bifunctional substituents (Ph —N—N —Ph and Me —N—CO —N—Me) are employed for the first time as protect-ing groups to block one or two PCl-functions in C1T—CIL—PCI-,. Cleavage of the PN-bonds in the five membered ring systems RP-CH 2 -PR-N(Ph)-N (Ph) (R = Me. Ph) with HCl affords the P-substituted methylenebis-chlorophosphanes RC1P—CH 2 — PC1R in satisfactory yields. The compounds have been characterized by 'H. I3 C{ 'H} and 3! F*{'H}NMR spectroscopy. With-in homologous substitution series of methylenebisphosphanes, e.g. R 2 P—CH 2 —PR 2 _"H" the coupling constants 2 /(PP) seem to reflect conformational changes at the PCP-skeleton. | | | |
Reference
| (Z. Naturforsch. 43b, 31—44 [1988]; eingegangen am 15. Juni 1987) | | | |
Published
| 1988 | | | |
Keywords
| Functional Methylenebisphosphanes Bifunctional Protecting Groups, Lithium and Trimethylsilyl Derivatives, Dynamic Li-Exchange, NMR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0031.pdf | | | | Identifier
| ZNB-1988-43b-0031 | | | | Volume
| 43 | |
| 113 | Author
| Frank Edelmann, Claudia Spang, HerbertW. Roesky, PeterG. Jones | Requires cookie* | | | Title
| Synthese und Struktur des ersten dreigliedrigen Arsen—Phosphor—Platin-Ringes Synthesis and Structure of the First Three-Membered Ring Containing Arsenic, Phosphorus and Platinum | | | | Abstract
| -butylphenylphosphane reacts with CpFe(C,H4AsCl2) in the presence of DBU to yield CpFe[C5H4As=PC6H2(f-Bu)?l. The reaction of this arsaphosphene with (Ph3P)2PtC2H4 yields CpFe[C5H4As—P[C6H2(r-Bu)3]Pt(PPh3)2], a compound with a three-membered ring containing arsenic, phosphorus and platinum. | | | |
Reference
| Z. Naturforsch. 43b, 517—520 (1988); eingegangen am 5. Januar 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, NMR Spectra, Phosphorus, Arsenic, Platinum 2, 4, 6-Tri | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0517.pdf | | | | Identifier
| ZNB-1988-43b-0517 | | | | Volume
| 43 | |
| 115 | Author
| Fritz Preuss, Harald Becker, Jürgen Kaub, WilliamS. Sheldrick | Requires cookie* | | | Title
| Darstellung und Struktur der zweikernigen tert-Butyliminovanadium(IV)-Komplexe: [('C 4 H 9 N) 2 V 2 Cp 2 X 2 ] (X = 0'C 4 H 9 , Cl) Synthesis and Molecular Structure of the Binuclear terf-Butyliminovanadium(IV) Complexes: [('C 4 H9N) 2 V 2 Cp 2 X 2 ] (X = O f C 4 H 9 , Cl) | | | |
Reference
| Z. Naturforsch. 43b, 1195—1200 (1988); eingegangen am 18. Februar 1988 | | | |
Published
| 1988 | | | |
Keywords
| ferr-Butylimino-cyclopentadienylvanadium(IV) Complexes, Preparation, X-Ray, NMR Spectra, ESR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1195.pdf | | | | Identifier
| ZNB-1988-43b-1195 | | | | Volume
| 43 | |
| 116 | Author
| Jörn Müller, Ke Qiao, Regina Schubert, M. Atthias Tschampel | Requires cookie* | | | Title
| ;r-01efin-Iridium-Komplexe, XVIII [1] Reaktionen von Bis[cycloocta-l,5-dien-//-chloro-iridium] mit w-Propyllithium in Gegenwart von Alkinen yr-Olefin Iridium Complexes, XVIII [1] Reactions of Bis[cycloocta-l,5-diene-/z-chloro-iridium] with n -Propyllithium in the Presence of Alkynes | | | | Abstract
| The reaction of [(cod)IrCl]2 (cod = //4-cycloocta-l,5-diene) with n-C3H7Li gives non-isola-ble (cod)IrH species by /3-elimination of (cod)Ir-n-C3H7 intermediates; the stable final prod ucts of further reactions with RC = CR highly depend on the nature of the substituents R. With R = Me the 6-endo-H-hexamethylcyclohexadienyl complex 1 is obtained together with the iridacyclopentadienyl compound 2 and known }[(cod)IrH]4C3H4} (3). In case of R = Et steric effects cause transfer of the hydridic hydrogen to the cod ligand, and the hexaethyl-benzene species 4 is isolated which was characterized by crystal structure analysis. The reac tion system with tolane again yields a 6-enJo-H-cyclohexadienyl complex (5). In all cases free substituted benzenes are formed as cyclotrimerization products of the alkynes. | | | |
Reference
| Z. Naturforsch. 48b, 1558—1564 (1993); eingegangen am 15. Juli 1993 | | | |
Published
| 1993 | | | |
Keywords
| Substituted Benzene, Cyclohexadienyl and Iridacyclopentadienyl Complexes, Synthesis, NMR Spectra, Crystal Structure | | | |
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| default:Reihe_B/48/ZNB-1993-48b-1558.pdf | | | | Identifier
| ZNB-1993-48b-1558 | | | | Volume
| 48 | |
| 117 | Author
| JensR. Goerlich, Axel Fischer, PeterG. Jones, Reinhard Schmutzler+ | Requires cookie* | | | Title
| Organophosphorverbindungen mit tertiären Alkylsubstituenten. III*: Synthese und Reaktionen Di-l-adamantylsubstituierter Phosphorverbindungen; Kristallstruktur von Di-l-Adamantylphosphinsäurechlorid Organophosphorus Compounds with Tertiary Alkyl Substituents. Ill: Synthesis and Reactions of D i-l-adam antyl-Substituted Phosphorus Compounds; Crystal Structure of Di-l-adam antylphosphinic Chloride | | | | Abstract
| The reaction of adamantane with PC13/A1C13, followed by hydrolysis, gave (l-Ad)2P(: 0)C1 1, which was converted to (l-Ad)2P(:Ö)F 2 and (l-Ad)2P(:S)Cl 3 by standard procedures. The structure of 1 was confirmed by a single crystal X-ray structure determination; despite the bulky substituents the P-C bond lengths are normal (184.0(3), 185.0(3) pm). Whereas chlorine-fluorine exchange in 3 with AsF3 furnished (l-Ad)2P(: S)F 4, desulfuration of 3 with Ph3P to give (l-Ad)2PCl 5 failed. The secondary phosphine oxides R 'R 2P(:0)H (R1, R2 = 1-Ad: 6; R1 = 1-Ad, R2 = 'Bu: 7; R1, R2 = 'Bu: 8) were synthesized by reaction of 1, l-AdP(:0)Cl2 and 'BuP(:0)Cl2 with 'BuLi. 6 and 8 reacted readily with chloral to give the adducts R2P(:0)CH(0H)CC13 (R = 1-Ad: 9; R = 'Bu: 10). Silylation of 6 with Me2NSiMe3 in the presence of dry air led to (l-Ad)2P(:0)0SiM e3 11, which was hydrolyzed to give (l-Ad)2P (:0)0H 12. (l-Ad)2POSiMe3 13 was obtained by the reaction of 6 with /z-BuLi, followed by Me3SiCl. No reaction took place upon heating 6 with Mo(CO)6. (l-Ad)2PCl 5 was synthesized in low yield by the reaction of 6 with PC13. The action of tetrachloro-o-benzoquinone (TOB) upon 6 furnished (l-Ad)2P(: 0)(o-OH)C6Cl4 15, whereas the 'butyl analogue of 15, 16, was synthesized by hydrolysis of the TOB-adduct of di-'butylfluorophos-phine. Analogous 1-adamantyl-and 'butyl-phosphorus compounds are compared with regard to their 31P NMR data. | | | |
Reference
| Z. Naturforsch. 49b, 801—811 (1994); eingegangen am 17. Dezember 1993 | | | |
Published
| 1994 | | | |
Keywords
| Di-l-adamantyl Phosphorus Compounds, Secondary Phosphine Oxides, Di-l-adamantyl Phosphinic Acid, NMR Spectra, X-Ray | | | |
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| default:Reihe_B/49/ZNB-1994-49b-0801.pdf | | | | Identifier
| ZNB-1994-49b-0801 | | | | Volume
| 49 | |
| 118 | Author
| Peter Dierkes, Gerlinde Frenzen, Sigrid Wocadlo, W. Erner Massa, Stefan Berger, Jürgen Pebler, Kurt Dehnicke | Requires cookie* | | | Title
| Komplexe des Typs [MCl4(SEt2)2] mit M = Mo und W. Kristallstrukturen, NMR-Spektren und magnetisches Verhalten [MCl4(SE t2)2] Complexes with M = Mo and W. Crystal Structures, NMR Spectra, and Magnetic Behaviour | | | | Abstract
| The crystal structures of the thioether complexes [MCl4(SEt2)2] with M = Mo and W have been solved by X-ray methods. Both compounds crystallize isotypically in the triclinic space group P I with two formula units per cell unit. The metal atoms are octahedrally coordinated by four chlorine atoms and by the two sulfur atoms of the thioether molecules in trans position (symmetry Q) with bond lengths (average): M o -C l 233.1, M o -S 253.4, W -C l 233.1, and W -S 251.7 pm. Both complexes were also characterized by !H and 13C NM R spectro scopy as well as by measurement of the magnetic susceptibilities in the tem perature range from 1.8 to 350 K. | | | |
Reference
| Z. Naturforsch. 50b, 159—167 (1995); eingegangen am 23. August 1994 | | | |
Published
| 1995 | | | |
Keywords
| D iethylthioethers of Molybdenum and Tungsten, Crystal Structure, NMR Spectra, Magnetic Susceptibility | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0159.pdf | | | | Identifier
| ZNB-1995-50b-0159 | | | | Volume
| 50 | |
| 119 | Author
| FredR. Oschea, G. Ernot, H. Eckm, Anna, FrankW. Ellerb, Ekkehard Fluck0 | Requires cookie* | | | Title
| Ein neuer Heterocyclus | | | | Abstract
| , 2A3,4A5-[l,2,4]-O xadiphosphinin (2), als Ligand eines zw eikernigen Eisenkom plexes A New H eterocycle, 2A3,4A5-[l,2,4]-O xadiphosphinine (2), as L igand o f a Binuclear Iron C om plex Preparation and properties of a coordination compound are described, in which a carbonyl group in bis[(dicarbonyl)(/;;i-cyclopentadienyl)iron] is substituted by hitherto unknown octa-Af-methyl-2A',4A:i-[l,2,4]-oxadiphosphinine-2,4,4,6-tetramine (2). The 'H , '1P, and l3C NMR spectra are recorded and discussed in detail. The molecular structure of the iron complex 4 is described and interpreted. | | | |
Reference
| Z. Naturforsch. 51b, 1725—1731 (1996); eingegangen am 27. Juni 1996 | | | |
Published
| 1996 | | | |
Keywords
| [l, 2, 4]-Oxadiphosphinine, Binuclear Iron Complex, NMR Spectra, X-Ray | | | |
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| default:Reihe_B/51/ZNB-1996-51b-1725.pdf | | | | Identifier
| ZNB-1996-51b-1725 | | | | Volume
| 51 | |
| 120 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| Synthese und Reaktivität von 7-Triphenylstannyl-a-am inobuttersäure- derivaten | | | | Abstract
| Ph3SnCH2CH 2C H (NHCOOCH 2P h)COOCH3 (1) is synthesized by hydrostannation of methyl N-(benzyloxycarbonyl)vinylglycinate with Ph3SnH. The reaction o f 1 with HC1 in CH 3OH and with bromine in CHC13 yields the halostannylsubstituted compounds Ph3_"X,?SnCH2CH 2C H(NHCOOCH 2Ph)C OOCH3 (2 -4) (n = 1, 2; X = Cl, Br). By sapo nification with one equivalent of NaOH and subsequent acidification with HCl 1 is transformed into the free acid Ph3SnCH2C H 2C H(NHCOOCH2Ph)COOH (5) that undergoes cyclization into the 1,2-oxastanninane 6 with intramolecular elimination of benzene. IR, NMR data and the determination of the crystal structure of Ph2BrSnCH2CH2CH(NHCOOCH2Ph)COOCH3(3) reveal for 2 and 3 an intramolecular coordination of the N C (0)0-group at the tin atom to form a seven-membered ring. | | | |
Reference
| (Z. Naturforsch. 52b, 9—16 [1997]; eingegangen am 20. August 1996) | | | |
Published
| 1997 | | | |
Keywords
| Triphenylstannyl Aminobutyric Acid Derivatives, Halostannyl Aminobutyric Acid Derivatives, IR Spectra, NMR Spectra, X-Ray | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0009.pdf | | | | Identifier
| ZNB-1997-52b-0009 | | | | Volume
| 52 | |
|
