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1997[X]
21Author    Michael Gerster, Martin Maier, Nils Clausen, Jens Schewitz, Ernst BayerRequires cookie*
 Title    Optimized Large Scale Synthesis of Phosphorothioate Oligonucleotides on PS-PEG Supports  
 Abstract    Sulphurization is a crucial step during synthesis of phosphorothioate oligonucleotides. Insuf­ ficient reaction leads to inhomogeneous products with phosphodiester defects and subsequently to destabilization of the oligomers in biological media. To achieve a maximum extent of sulphur incorporation, various sulphurizing agents have been investigated. Solely, the use of Beaucage reagent provided satisfactory results on PS-PEG supports. Based on our investigations in small scale synthesis (1 //mol) with continuous-flow technique, upscaling to the 0.1-0.25 mmolar range has been achieved using a peptide synthesizer. The syntheses were performed in batch mode with standard phosphoramidite chemistry. Additionally, large scale synthesis of a phos­ phodiester oligonucleotide has been carried out on PS-PEG with optimized protocols and compared to small scale synthesis on different supports. Products were analysed by 31P NMR, capillary gel electrophoresis and electrospray mass spectrometry. An extent of sulphurization of 99% and coupling effiencies of more than 99% were obtained and the products proved to have similar purity compared to small scale syntheses on CPG. 
  Reference    (Z. Naturforsch. 52b, 110—116 [1997]; received September 11 1996) 
  Published    1997 
  Keywords    Large Scale Synthesis, Oligonucleotide Phosphorothioate, PS-PEG, Sulphurizing Reagent 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0110.pdf 
 Identifier    ZNB-1997-52b-0110 
 Volume    52 
22Author    Z. NaturforschRequires cookie*
 Title    Synthesis of Cationic Ruthenium Thioketene Complexes through Intramolecular 1,2-Elimination [1]  
 Abstract    Halfsandwich thiocarboxylate complexes [CpRu(PR3)->(SC(0)CH2R')] ((P R 3)2 = (PPh3)2, Ph2PCH 2PPh2 (dppm), Ph2PC2H4PPh2 (dppe); R' = C6H 5, 4-C6H4Me, 4-C6H 4OMe, 4-C6H4C1) are obtained from the corresponding thiolate complexes [CpRu(PR3)2SH] and acyl chlorides. The structure of [CpRu(dppm)(SC(0)CHTPh)] was determined: monoclinic space group P2j/c (No. 14), a = 9.229(2), b = 16.680(3),"c = 21.447(5)Ä, ß = 90.751(12)°, Z = 4. Reaction of the thiocarboxylate complexes with the anhydrides of either trifluoro-acetic acid or trifluoromethanesulfonic acid gives thioketene complexes [CpRu(dppm) (?;2-S=C=CHR')]PF(s. H ie structure of [CpRu(dppm)0/2-S= C = C H Ph)]PF6 was deter­ mined: monoclinic space group P2,/c (No. 14), a -13.814(5), b -15.338(2), c = 17.057(7) Ä, ß = 93.74(2)°, Z = 4. 
  Reference    (Z. Naturforsch. 52b, 117—124 [1997]; received July 25 1996) 
  Published    1997 
  Keywords    Ruthenium Complexes, Thiocarboxylate, Thioketene, Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0117.pdf 
 Identifier    ZNB-1997-52b-0117 
 Volume    52 
23Author    RolfW. Saalfrank3, Roland Harbig3, Oliver Struck, Frank Hampel3, Eva Maria Petersc, Karl Petersc, HansG. Eorg, Von SchneringcRequires cookie*
 Title    Eindimensionale Kupfer(II)-Koordinationspolymere: Kristall-Engineering durch variable Verknüpfungsmuster [1] One Dimensional Copper(II) Coordination Polymers: Crystal Engineering through Variable Types of Linkage [1]  
 Abstract    of a methanolic copper(II) acetate solution with tetrazolyl enol derivatives 2a or 2b leads to the formation of the corresponding lD-coordination polymer ^[CuL2] 3a and pseudo lD-coordination polymer [CuL2]2 3b, respectively. On the contrary, reaction of 2c with methanolic copper(II) acetate solution yields OH-bridged lD-coordination polymer ^[CuL2(MeOH)2l 3c. Single-crystal X-ray diffraction of the supramolecular species 3 established unequivocally the structures of the stairlike coordination compounds. Reaction of a methanolic copper(II) acetate solution with amidotetrazole derivative 6 leads to the formation of the lD-coordination polymer ^,[CuL2] 7. The structure of 7 has been established by X-ray structure analysis. 
  Reference    (Z. Naturforsch. 52b, 125—134 [1997]; eingegangen am 6. August 1996) 
  Published    1997 
  Keywords    Tetrazolyl Enols, Coordination Polymers ID, Copper Complexes, Self-Assembly, Crystal Engineering Reaction 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0125.pdf 
 Identifier    ZNB-1997-52b-0125 
 Volume    52 
24Author    R. Olf, M. Inkwitz, Jens JakobRequires cookie*
 Title    D arstellung und spektroskopische Charakterisierung von T rifluorm ethylazosulfonylm ethan C H 3S ( 0 ) 2N N C F 3 P rep aratio n and Spectroscopic C haracterization of Trifluorom ethylazosulfonylm ethane C H 3S ( 0 ) 2N N C F  
 Abstract    The reaction of trifluoronitrosomethane with CH3S (0)2NH2 and Na2C 0 3 as a base in THF gi­ ves the yellow liquid CH3S (0)2NNCF3, m.p. 18 °C, which was characterized by vibrational and NMR spectra. 
  Reference    Z. Naturforsch. 52b, 135—137 (1997); eingegangen am 21. Oktober 1996 
  Published    1997 
  Keywords    Trifluoromethylazosulfonylmethane, Preparation, Vibrational Spectra, NMR Spectra 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0135_n.pdf 
 Identifier    ZNB-1997-52b-0135_n 
 Volume    52 
25Author    FrankK. Unkel, K. Laus, H. Arm, KurtD. EhnickeRequires cookie*
 Title    Kristallstruktur  
 Abstract    -Trichloro-c y c lo -li6-wolfram a-3,5-dithia-2,4,6-triazin, [W C 13(N 3S2)]2 C rystal S tructure of 1,1,1-Trichloro-cyclo-126-tungsta-3,5-dithia-2,4,6-triazine, [WC13(N 3S2) ] 2 Tungsta-dithia-triazine, Crystal Structure Single crystals of [WC13(N3S2)]2 were obtained by the reaction of triphenyl-cyclo-lA5-antimonia-2,4-dithia-3,5-diazine, SbPh3(N2S2), with tungsten hexachloride in dichloromethane. Space group 
  Reference    Z. Naturforsch. 52b, 138—140 (1997); eingegangen am 17. September 1996 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0138_n.pdf 
 Identifier    ZNB-1997-52b-0138_n 
 Volume    52 
26Author    R. Ainer PöttgenRequires cookie*
 Title    T he Stannide Zr5CuSn3  
 Abstract    Crystal Structure, Zirconium Copper Stannide Zr5CuSn3 was prepared from the elements in an arc-melting furnace and investigated by X-ray diffraction of powders as well as of single crystals. The crystal structure was refined from four-circle diffractometer data: P63/mcm, a = 860.04(7) pm, c -586.80(5) pm, V = 0.3759(1) nm3, Z = 2, wR2 = 0.0402 for 371 F2 values and 15 variables. A refinement of the occupancy parameters re­ vealed that the copper position is occupied to only 95.3(8)% in the crystal used for the X-ray investigation. Zr5CuSn3 crystallizes in the Hf5CuSn3 type structure, a filled variant of the Mn5Si3 type. The main features of the Zr5CuSn3 structure are condensed Zr6 octahedra that are centered by copper atoms. 
  Reference    Z. Naturforsch. 52b, 141—144 (1997); received September 19 1996 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0141_n.pdf 
 Identifier    ZNB-1997-52b-0141_n 
 Volume    52 
27Author    Z. NaturforschRequires cookie*
 Title      
 Abstract    Single crystals of (Me3Sn)3CCN were obtained by the reaction of tris(trimethylstannyl)amine with boiling acetonitrile in the presence of potas­ sium fluoride and trimethylarsane. The compound has been characterized by IR spectroscopy and by a crystal structure determination. Space group 
  Reference    Z. Naturforsch. 52b, 145—148 (1997); eingegangen am 7. Oktober 1996 
  Published    1997 
  Keywords    Tin Compound, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0145_n.pdf 
 Identifier    ZNB-1997-52b-0145_n 
 Volume    52 
28Author    Z. NaturforschRequires cookie*
 Title      
 Abstract    The crystal structures of PbMe3I and BiPh2Cl have been determined by X-ray methods. Both compounds form polymeric chains via bent [i2-ha-logeno bridges and almost linear X-M-X units (X = I, Cl). 
  Reference    Z. Naturforsch. 52b, 149—152 (1997); eingegangen am 20. September 1996 
  Published    1997 
  Keywords    Lead, Bismuth Compounds, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0149_n.pdf 
 Identifier    ZNB-1997-52b-0149_n 
 Volume    52 
29Author    Y. Grina, Hk Müller-Buschbaum, H. G. Von Schnering3Requires cookie*
 Title    "BaNb3 0 6" ist ein Perowskit BaNbC>3 , eine Korrektur und ein Beitrag zu BajcNb0 3 "BaNb30 6" is a Perovskite B a N b 0 3, a Correction and a Contribution to BavN b 0 3  
 Abstract    Barium Niobium Oxide It is shown that the trigonal compound "BaNb30 6" described earlier actually is the cubic perovskite BaN b03 with an unusually small lattice constant of 4.039 A. Furthermore, the refinement of the single crystal data prepared by C 0 2-LASER techniques did not reveal defects at the Ba position, but defects at the positions of niobium and oxygen, corresponding to the composition Ba(NbO3)0 9 or Ba, 08NbO3. 
  Reference    Z. Naturforsch. 52b, 153—156 (1997); eingegangen am 30. September 1996 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0153.pdf 
 Identifier    ZNB-1997-52b-0153 
 Volume    52 
30Author    Ayhan Elmali3, Yalcin Elermana, Ingrid Svobodab, Hartmut Fuessb, Klaus Griesar0, Wolfgang HaasecRequires cookie*
 Title    Structure and Magnetic Properties of a Dinuclear Copper(II) Complex  
 Abstract    [Cu2L] (L=N-2-hydroxy-4-methylphenyl-4-oxo-2-pentalketimine) was synthesized and its crystal structure determined. C24H?6Cu2N204 monoclinic space group P2|/n with a= 10.978(2), 17.045(3), c= 11.958(2) Ä, ß = 101.89(1)°, V = 2189.6(7) A3,Z = 4. Two copper(II) atoms in a distorted square-planar coordination are bridged by two oxygen atoms to form a dinuclear unit. The copperfll) centers are separated by 3.025(1) A and antiferro-magnetically coupled (7=-222.3 cm), which follows from temperature-dependent magnetic susceptibility measurements in the range 4.2 to 300 K. 
  Reference    Z. Naturforsch. 52b, 157—161 (1997); received September 30 1996 
  Published    1997 
  Keywords    Dinuclear Cu(II) Complex, X-Ray, Structure, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0157.pdf 
 Identifier    ZNB-1997-52b-0157 
 Volume    52 
31Author    Hans-Peter Schrödel, Alfred SchmidpeterRequires cookie*
 Title    Phosphorandiyl-l,3,5-triphosphinane/ Phosphonio-l,3,5-triphosphinin Kationen Phosphoranediyl-l,3,5-triphosphinanes / Phosphonio-l,3,5-triphosphinine Cations  
 Abstract    Depending on the reaction conditions, the condensation of triphenylphosphonium bis(trimethylsilyl)methylide 1 with phosphorus trichloride and phosphorus tribromide gives the cyclic trimers (Ph3P=CP-X)3, X = Cl, Br, trihalo-tris(triphenylphosphoranediyl)-1,3,5-triphosphinanes 3 and 5. In solution the compounds dissociate to give the ionic forms 4 and 6 which rapidly exchange the halide between the halophosphine and the phosphenium moieties. The exchange is slowed down when the halide ion is replaced by a tosylate ion. Substitution of the covalent chloride of 4 for diphenylphosphino groups gives again an ionic product 10, while the introduction of a morpholino group as well as the replacement of all chloride by triflate give dicationic compounds 12 and 13. Reaction of 3 with gallium trichloride finally leads to the tris(triphenylphosphonio)-l,3,5-triphosphinine trication as a major equilibrium participant. 
  Reference    Z. Naturforsch. 52b, 162—168 (1997); eingegangen am 24. Oktober 1996 
  Published    1997 
  Keywords    Phosphonium Ylides, Halophosphines, Phosphenium Ions, 1, 3, 5-Triphosphinines, Halide Exchange 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0162.pdf 
 Identifier    ZNB-1997-52b-0162 
 Volume    52 
32Author    M. Wachhold, W. S. SheldrickRequires cookie*
 Title    Methanolothermale Synthese von Rb3AsSe4 * 2 Se6 und Cs3AsSe4 * 2 Cs2As2Se4 * 6 Te4Se2, zwei Selenidoarsenate mit sechsgliedrigen Chalkogenringen Methanolothermal Synthesis o f Rb3A sSe4 * 2 Se6 and Cs3AsSe4 * 2 Cs2A s2Se4 * 6 Te4Se2. Two Selenidoarsenates with Six-Membered Chalcogen Rings  
 Abstract    The methanolothermal reaction of Rb2C 0 3 with As2Se3 and black selenium leads to the formation of Rb3AsSe4 and the new selenidoarsenate(V) Rb3AsSe4 • 2 Se6 (1), which crys­ 
  Reference    Z. Naturforsch. 52b, 169—175 (1997); eingegangen am 29. Juli 1996 
  Published    1997 
  Keywords    Selenium, Tellurium, Ring Systems, Selenidoarsenate, Methanolothermal Synthesis 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0169.pdf 
 Identifier    ZNB-1997-52b-0169 
 Volume    52 
33Author    ThorstenM. Gesinga, KlausH. Wachtmannb, Wolfgang JeitschkoRequires cookie*
 Title    The Perovskite Carbides A3MC (A = Sc  
 Abstract    Crystal Structure, Perovskite Carbides Twentyfive new perovskite carbides have been obtained either by arc-melting cold-pressed pellets of the elemental components with subsequent annealing at 900 °C or by heating stoichio­ metric quantities of the elements in a high-frequency furnace. Also, thirtyseven compounds of this structure type are confirmed and their lattice constants are reported. The crystal structures of SC3MC (M = Al, Ga, In, Tl) were refined from X-ray powder data, and in all cases only the octahedral voids formed by scandium atoms were found to be fully occupied. The hydrolysis of the carbides Sc^GaC, Y3SnC, YjPbC and Ho3PbC with diluted hydrochloric acid resulted in about 84 -97 (wt-)% methane and 3 -16 % saturated and unsaturated higher hydrocarbons. The cell volumes of the ternary carbides A3MC and the corresponding binary Cu3Au type compounds A3M are compared and several inconsistencies are pointed out. 
  Reference    Z. Naturforsch. 52b, 176—182 (1997); received August 6 1996 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0176.pdf 
 Identifier    ZNB-1997-52b-0176 
 Volume    52 
34Author    O. V. Quinzania, S. Tarullia, O. E. Pirob, E. J. Baranc, E. E. Castellano0Requires cookie*
 Title    Crystal Structure, Vibrational Spectra and Thermal Analysis of Bis(saccharinato)bis(pyridine)zinc(II)  
 Abstract    The crystal structure of [Zn(sac)2(py)2] has been de termined by single-crystal X-ray diffrac-tometry. It crystallizes in the monoclinic space group C2/c with Z = 4. We propose and discuss an assignment of its IR and Raman spectra, compatible with the structural characteristics. Its thermal behavior was investigated by means of TG and DTA methods. Some comparisons with related compounds are made. 
  Reference    Z. Naturforsch. 52b, 183—187 (1997); received July 1 1996 
  Published    1997 
  Keywords    Zinc, Saccharin/Pyridine, Crystal Structure, IR Spectra, Raman Spectra 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0183.pdf 
 Identifier    ZNB-1997-52b-0183 
 Volume    52 
35Author    Stefan Dick, Armin WeissRequires cookie*
 Title    Neue dreizähnige Liganden vom Typ N-AlkyI-N,N-bis(2-pyridylmethyl)amin New Tridentate Ligands of the Type N-Alkyl-N,N-bis(2-pyridylmethyl)amine  
 Abstract    New tridentate ligands of the type N-alkyl-N,N-bis(2-pyridylmethyl)amine (alkyl = me­ thyl, benzyl, adamantyl) have been synthesized by reaction of alkylamines with 2 -(chlor-methyl)pyridine in alkaline solution. These amines are preferably isolated and stored as per­ chlorates. The perchlorate of the methyl substituted ligand has been crystallized in two modifi­ cations that differ in the twisting of the aromatic rings and in the coordination of the perchlorate anions. 
  Reference    Z. Naturforsch. 52b, 188—192 (1997); eingegangen am 1. August 1996 
  Published    1997 
  Keywords    Tridentate Amine, Perchlorate Salt, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0188.pdf 
 Identifier    ZNB-1997-52b-0188 
 Volume    52 
36Author    Requires cookie*
 Title    Uber die Reaktion von SbPh3 mit S3N2CI2 Kristallstrukturen von [Ph3SbSNSN] und [(P h jS b C ^ fe ^ N J  
  Reference    Z. Naturforsch. 52b, 193 (1997) 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0193.pdf 
 Identifier    ZNB-1997-52b-0193 
 Volume    52 
37Author    Amo Pfitzner, Eva FreudenthalerRequires cookie*
 Title    (CuI)2Pi4* ein neues Phosphorpolymer in einer Kupferhalogenid-Matrix (CuI)2P 14: a Novel Phosphorus Polymer in a Copper Halide Matrix  
 Abstract    (CuI)2Pi4 is a new adduct of copper iodide to a neutral phosphorus polymer. It is obtained by reaction of Cul and Pred at 400 °C. The compound crystallizes monoclinically, space group P2,/c (No. 14), a = 9.919(2), b = 9.718(2), c = 16.478(3) Ä, ß = 105.71(1)°, V = 1529.0(7) A3, with Z = 4. The crystal structure was refined to R\ = 0.029 for 2680 reflections and 173 parameters. It contains a new polymeric phosphorus allotrope with the translational unit P^° consisting of experimentally unknown [PI2] groups which are linked by [P2] fragments. The phosphorus rods consist of five-and six-membered rings, and are coordinated only by copper atoms. 
  Reference    Z. Naturforsch. 52b, 199—202 (1997); eingegangen am 11. September 1996 
  Published    1997 
  Keywords    Phosphorus, Copper Compounds, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0199.pdf 
 Identifier    ZNB-1997-52b-0199 
 Volume    52 
38Author    M.Elena Olmos, Annette Schier, Hubert SchmidbaurRequires cookie*
 Title    2-(Diphenylphosphino)-pyridine as an Ambidentate Ligand in Homo-and Hetero-binuclear Complexes of Copper, Silver, and Gold  
 Abstract    Copper(I), Silver(I), Gold(I) Coordination, 2-(Diphenylphosphino)-pyridine, 1-Pyridyl-diphe-nylphosphine, Ambidentate Ligand The reaction of 2-diphenylphosphino-pyridine (1) with AgBF4 in an equimolar ratio affords 
  Reference    Z. Naturforsch. 52b, 203—208 (1997); received December 12 1996 
  Published    1997 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0203.pdf 
 Identifier    ZNB-1997-52b-0203 
 Volume    52 
39Author    JoséM. López-De-Luzuriaga, Marcus Söldner, Annette Schier, Hubert SchmidbaurRequires cookie*
 Title    Gold(I) Complexes of Open-chain and Cyclic Di-secondary Amines  
 Abstract    Treatment of N,N'-diisopropyl-ethylenediamine or 1,4-piperazine with two equivalents of [(Ph^P)Au]+ BF4-leads to binuclear complexes of the diamines: {[(Ph3P)Au]HN('Pro)NCH2-}22+ 2 BF4~ (1) and {[(Ph3P)Au]HNCH2CH2}22+ 2 BF4~ (2), respectively. In the products each quaternary ammonium center bears one gold ligand, one hydrogen atom and two alkyl substituents. The crystal structures of both compounds have been determined. Compound 1 contains discrete ion-triples. The ethylene bridge in the dications is in an unfolded conformation, with a crystallographic center of inversion, and allows for weak hydrogen bonding N-H--F [2.085 A; N-H--F 169.2°] between the NH functions and the counterions. The existing distant contacts F-A u [3.599 A] are probably less significant for the aggregation of the ion triples, but will contribute through Coulomb forces. Compound 2 crystallizes with two solvent molecules CH2CI2. The dication has a crystallographic center of inversion with the piperazine ring in a chair conformation and the gold atoms in equatorial positions. There are hydrogen bonds N-H--F [2.076 and 2.457 A] between the dication and the anions which lead to the formation of ion-triples, with further contacts between the BF4~ anions and the solvent molecules [C-H--F 2.340 and 2.446 A]. 
  Reference    Z. Naturforsch. 52b, 209—213 (1997); received December 4 1996 
  Published    1997 
  Keywords    Gold(I) Coordination, Amine Complexes, Secondary Amines, Ammonium Complexes 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0209.pdf 
 Identifier    ZNB-1997-52b-0209 
 Volume    52 
40Author    Horst Kunkely, Amd VoglerRequires cookie*
 Title    Photoreactivity of Coordinated Phenylhydrazine. Intraligand Excitation of ReCl(CO)3(PhNH-NH2)2  
 Abstract    The complex of ReCl(CO)3(PhNH-NH2)2 shows an absorption band at A max = 272 nm which is assigned to an IL (intraligand) transition of the coordinated phenylhydrazine. Upon IL excitation the complex undergoes a decomposition with 4> = 0.03 at Ajrr = 280 nm. 
  Reference    Z. Naturforsch. 52b, 214—216 (1997); received September 20 1996 
  Published    1997 
  Keywords    Rhenium Complexes, Phenylhydrazine Complexes, Photochemistry 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0214.pdf 
 Identifier    ZNB-1997-52b-0214 
 Volume    52 
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