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1998[X]
61Author    Requires cookie*
 Title    The Molecular Structures and Conformational Preferences of Bis(dimethylstibyl)-Sulfane and -Tellurane, E(SbMe2)2? E = S or Te, Me = CH3, by Density Functional Theory Calculations and Gas Electron Diffraction  
  Reference    Z. Naturforsch. 53b, 381 (1998) 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0381.pdf 
 Identifier    ZNB-1998-53b-0381 
 Volume    53 
62Author    Z. NaturforschRequires cookie*
 Title    Experimental and Computational Studies on Aminoguanidine Free Base, Monocation and Dication. Part III: Proton Affinities of Guanidine, Aminoguanidine and Glyoxal Bis(amidinohydrazone)  
 Abstract    The structures of glyoxal bis(amidinohydrazone) (GBG) free base and glyoxal bis(amidi-nohydrazonium) monocation and dication were calculated quantum chemically by using the density functional hybrid method B3-LYP with the standard basis set 6 -3 1 G (d). Proton affinities calculated from these data are 246.4 kcal/mol for the free base and 176.0 kcal/mol for the monocation. The proton affinities of guanidine free base (246.2 kcal/mol), am inogua­ nidine free base (242.9 kcal/mol), aminoguanidinium monocation (88.6 kcal/mol) were calcu­ lated for reference. The B3-LYP functional overestimates the proton affinities for all the species studied. For example, for guanidine the proton affinity at the M P2/6-31G (d) level is 238.3 kcal/mol, the experimental reference value being 233 kcal/mol. However, from the B3-LYP values it can be concluded that in the gas phase all the three bases are nearly equally basic. On the other hand, it is known that in aqueous solution guanidine is a much stronger base than aminoguanidine and glyoxal bis(amidinohydrazone). The results are discussed from the point of view of molecular size, shape and symmetry, and hydrogen bonding in solution. 
  Reference    Z. Naturforsch. 53b, 386—392 (1998); received November 21 1997 
  Published    1998 
  Keywords    Proton Affinity, Gas Phase Basicity, Acid Dissociation Constant 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0386.pdf 
 Identifier    ZNB-1998-53b-0386 
 Volume    53 
63Author    Z. NaturforschRequires cookie*
 Title    R eaction o f 9-B orabicyclo[3.3.1]nonane with N-Trim ethylsilylam ines -C leavage o f the N-Si or N -H Bond  
 Abstract    The reaction of dimeric 9-borabicyclo[3.3.1]no-nane 1 with N-trimethylsilyl-aniline 2 affords 9-anilino-9-borabicyclo[3.3.1]nonane 5 by elimina­ tion of trimethylsilane. In contrast, 1 reacts with the N-trimethylsilyl-2-aminopyridines 3 and 4 se­ lectively by elimination of H 2 to give the corre­ sponding N-trimethylsilyl-aminoboranes 6 and 7. The latter reactions proceed via formation of bo-rane-pyridine adducts. 
  Reference    Z. Naturforsch. 53b, 393—395 (1998); received December 29 1997 
  Published    1998 
  Keywords    Aminoborane, Aminosilane, Boron, Pyridine, NMR Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0393_n.pdf 
 Identifier    ZNB-1998-53b-0393_n 
 Volume    53 
64Author    J. Feller3, H. Oppermann3, R. Kucharkowskib, S. DäbritzcRequires cookie*
 Title    Phasenbeziehungen und Chemischer Transport der Verbindungen im ternären System Re/Mo/O Phase Relations and Chemical Transport of the Compounds in the Ternary System Re/Mo/O  
 Abstract    In the ternary system Re/Mo/O four series of mixed oxides have been prepared by heating of powder samples and by transport reactions. The series are derived from the oxides R e 0 2, M o 0 2, 7 -Mo4O u und //-Mo40 |i and have compositions R e1_ vM ov0 2 (0 < x < 0.37), M o,_> .Re>0 2 (0 < v < 0 .4 2),7 -M o 4_-| Re-| 0 11 (0 < Zj < l),a n d /7-Mo4_.2Re-^Ö |, (0 < z 2 < 1). Contributions to the understanding of the transport mechanism were obtained from thermodynamic calculations. The composition of the mixed crystals obtained have been determined by EPM A and ICP-AES. 
  Reference    Z. Naturforsch. 53b, 397—104 (1998); eingegangen am 21. Januar 1998 
  Published    1998 
  Keywords    Rhenium Molybdenum Mixed Oxides, Chemical Transport Reaction, Phase Diagram 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0397.pdf 
 Identifier    ZNB-1998-53b-0397 
 Volume    53 
65Author    Matthias Asbrand, Brigitte Eisenmann, Holger Engelhardt, Ute RößlerRequires cookie*
 Title    Dimere und polymere Pnictidostannat(IV)-Anionen -Darstellung und Kristallstrukturen von Na2K3[SnP3], Na2Cs3 [SnP3] und Na2K3[SnBi3] Dimeric and Polymerie Pnictidostannate(IV) Anions -Preparation and Crystal Structures of Na2K3[SnP3], Na2Cs3[SnP3] and Na2K3[SnBi3]  
 Abstract    Disodium Tripotassium Triphosphidostannate(IV), Disodium Tricesium Triphosphidostanna-te(IV), Disodium Tripotassium Tribismutidostannate(IV), Dimeric Tetrahedral Anions, Zweier Single Chains The metallic lustrous compounds Na2K3[SnP3], Na2Cs3[SnP3], and Na2K3[SnBi3] were pre­ pared from melts of mixtures of the elements. The isotypic compounds Na2K3[SnP3] and Na7Cs3[SnP3] crystallize in the orthorhombic system, space group Cmca (No 64), Z = 8, with lattice constants a = 1996.1 (4)/2047.9(4) pm, b = 669.5(1)/686.5(2) pm, c = 1494.5(2)/1617.8(3) pm. The structure is characterized by dimeric units [Sn2P6] l0_ of edge-sharing [SnP4] tetrahe­ dra, which are coordinated by the alkali cations. Na2K3[SnBi3] crystallizes in the orthorhombic system, space group Ibca (No 73), Z = 8, with lattice constants a = 718.2(1) pm , b -1692.6(2) pm, c = 2159.5(2) pm. In the anionic partial structure [SnBi4] tetrahedra are connected via common corners to infinite ^ [SnBi3]5_ Zweier single chains. The sodium and potassium cat­ ions separate the chains from each other. Neglecting the distortions caused by covalent bonding and different radii both structure types can be classified as superstructure defect variants of the Li3Bi structure. Different orderings in the occupation of the tetrahedral voids lead to the variants in the anionic assemblies. 
  Reference    Z. Naturforsch. 53b, 405—410 (1998); eingegangen am 26. Januar 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0405 
 Volume    53 
66Author    Bernd Wrackmeyer, Ēriks Kupče+Requires cookie*
 Title    Some Applications of Ultrahigh Resolution 15N NMR Spectroscopy  
 Abstract    NMR Data, Ultrahigh Resolution Ultrahigh resolution l5N NM R spectra were measured for two nitroalkanes (M eNÜ2 la, fBuN02 lc), two isocyanates (;BuNCO 2c, Me^SiNCO 2d), four isothiocyanates (MeNCS 3a, EtNCS 3b, 'BuNCS 3c, M e3SiNCS 3d), one carbodiimide (Me3SiNCNSiM e3 4d), one keteneimine [Me3SiNCC(SiM e3)2 5d], two sulphinyl imides ('BuNSO 6c, M e3SiNSO 6d), and N-terf-butyl-pyrrole 7c, in order to determine coupling constants J (15N ,I3C) and isotope induced chemical shifts 1zAl2/13C (15N) at the natural abundance of the isotopes. The values 1 Z \I2/I3C (I5N) can be separated into two groups, one dealing with NC single and another one with NC double bonds. In each group (with few exceptions), the values 1A 2/13C (l5N) become more negative with a decrease in the absolute magnitude of l'7 (l5N ,13C)l. The corresponding values '2 r 4/l5N (l3C) show a sim ilar behaviour. However, N-substituted pyrroles appear to be exceptional in this respect. 
  Reference    Z. Naturforsch. 53b, 411—415 (1998); received January 26 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0411 
 Volume    53 
67Author    Matthias Biedermanna, Helmut Hartung3, Heinz Böhlandb, Regina MatthäusRequires cookie*
 Title    Koordinationsambidenz des Thiocyanations in Alkalitrithiocyanatomanganat(II)-Hydraten Coordination Ambidence of the Thiocyanate Anion in Alkali Trithiocyanatomanganate(II) Hydrates  
 Abstract    Alkali Thiocyanatomanganate(II) Hydrates, Crystal Structure, Coordination Ambidence Alkali metal trithiocyanatomanganate(II) hydrates have been prepared and characterized by several analytical methods. The structures of NH4[Mn(NCS)3(H20)] (la), K [M n(NCS)3(H20)] (lb) and Na[M n(NCS)3] • 3 H20 (2) could be elucidated by X-ray analysis, la and lb are isotypic and form a polymeric layer structure which is characterized by the ambident nature of the thiocyanate ligand and binding of the water molecule to the octahedrally coordinated Mn atom. In 2 the complex manganate(II) anions form a layer structure with trigonal symmetry in which each Mn atom is connected with three Mn neighbours by thiocyanate double bridges. The cation partial lattice consists of infinite chains of face-sharing [Na(H20) 6]+ octahedra running perpendicular to the anion layers. 
  Reference    Z. Naturforsch. 53b, 416—422 (1998); eingegangen am 28. Januar 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0416 
 Volume    53 
68Author    Horst Kunkely, Amd VoglerRequires cookie*
 Title    Charge Transfer Interaction in (Riboflavin)tricarbonylrhenium(I) Chloride  
 Abstract    Charge Transfer, Rhenium Complexes, Riboflavin [Re(riboflavin)(CO)3Cl] shows intraligand (Amax = 476 and 518 nm) and Re(I) to 7r* (riboflavin) metal-to-ligand charge transfer, MLCT, (Amax = 556 nm, in CH^CN) absorptions in close proximity. The MLCT band undergoes a moderate solvent-dependent shift (negative solvatochromism) indicating a partial charge separation in the excited state. The complex is not photoluminescent. 
  Reference    Z. Naturforsch. 53b, 423—425 (1998); received February 5 1998 
  Published    1998 
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 Identifier    ZNB-1998-53b-0423 
 Volume    53 
69Author    Rolf Minkwitz, Stefan SchneiderRequires cookie*
 Title    Die Tieftemperaturkristallstruktur von Trimethylsilanol The Low Temperature Crystal Structure of Trimethylsilanol  
 Abstract    A preparation of trimethylsilanol by hydrolysis of bis(trimethylsilyl)carbonate in diethylether at -2 0 °C is reported. At -8 0 °C, the crystals are monoclinic, space group P2,/c, Z = 12 with cell dimensions a = 996.0(2) pm, b = 1730.2(3) pm, c = 1122.9(2) pm, ß = 96,61(3)°. There are three independent Me3SiOH units with a slightly distorted tetrahedral C3SiO core structure. 
  Reference    Z. Naturforsch. 53b, 426 (1998); eingegangen am 5. Dezember 1997 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0426.pdf 
 Identifier    ZNB-1998-53b-0426 
 Volume    53 
70Author    GeraldL. Wegner, AlexanderJockisch Hubert SchmidbaurRequires cookie*
 Title    Synthesis and Structure of Benzyltriethylammonium Trichlorogermanate(II)  
 Abstract    Germanium Dichloride, Trichlorogermanate(II) The reaction of equimolar quantities of G eC h • dioxane with [BzEt3N]+ C P in tetrahydro-naphthaline gives high yields of [BzEt3N]+ [G eC h]~. The asymmetric unit of the monoclinic single crystals (from CH 2 CI2 , space group P2i/c, Z = 8) are comprising two pairs of crystallo­ graphically independent cations and anions, each with very similar molecular dimensions. The isolated [G eC b]-anions have a trigonal pyramidal structure with narrow Cl-Ge-Cl angles in the range from 93.41(5) to 98.27(5)° and Ge-Cl distances between 2.293(2) and 2.305(2) A. This structure is thus very similar to that of the isoelectronic A sCb molecule and of the [SeCl3 ]+ cation. 
  Reference    Z. Naturforsch. 53b, 430—33 (1998); received January 30 1998 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0430.pdf 
 Identifier    ZNB-1998-53b-0430 
 Volume    53 
71Author    Gabriele Korus, Martin JansenRequires cookie*
 Title    Kristallstruktur von Natriumtrifluormethylsulfonat- Trifluormethylsulfonsäure (1/3) Studies on Sodium Trifluoromethanesulfonate. Crystal Structure of Sodium Trifluoromethanesulfonate-Trifluoromethanesulfonic Acid (1/3)  
 Abstract    Single crystals of sodium trifluoromethanesulfonate-trifluoromethanesulfonic acid (1/3) (N aS 0 3CF3 • 3 H S 0 3CF3) have been prepared by reaction of sodium trifluoromethanesulfonate with anhydrous trifluoromethanesulfonic acid at 60 °C. N aS 0 3CF3 • 3 H S 0 3CF3 crystallizes in space group 1 2 ^ (No. 199) with a = 16.210(1) A, Z = 8. Sodium is coordinated by six oxygen atoms from six different trifluoromethanesulfonic acid molecules, each acid molecu­ le connecting two sodium ions. The 3-dimensional network resulting from the edge sharing octahedra corresponds to the cubic (10, 3) net, not realised otherwise, so far. The trifluorome­ thanesulfonate anion is bonded to three trifluoromethanesulfonic acid molecules by hydrogen bonds. 
  Reference    Z. Naturforsch. 53b, 438—442 (1998); eingegangen am 19. Dezember 1997 
  Published    1998 
  Keywords    Sodium Trifluoromethanesulfonate, Sodium Triflate, Trifluoromethanesulfonic Acid, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0438.pdf 
 Identifier    ZNB-1998-53b-0438 
 Volume    53 
72Author    Z. NaturforschRequires cookie*
 Title    Ein weiteres 2A5,4A5-Diphosphapyridin: 2,2,4,4-Tetrakis-(dimethylamino)-6- amino-l-aza-2A5,4A5-diphosphinin  
 Abstract    A Further 2A5,4A5-Diphosphapyridine: 2,2,4,4-Tetrakis-(dimethylamino)-6-amino-1-aza-2A5,4A5-diphosphinine.-(dimethylamino)-6-amino-l-aza-2A5,4A5-diphosphinine (3) has been pre­ pared by reacting l,l,3,3-tetrakis(dim ethylam ino)-lA 5-3A:'-diphosphete (1) with bis(trimethyl-silyl)carbodiimide (2) in a 2 : 1 molar ratio. Properties, 'H, P, and l3C NMR, mass, and IR spectra are reported and discussed. Com pound 3 is further characterized by X-ray structure analysis. 
  Reference    Z. Naturforsch. 53b, 443—147 (1998); eingegangen am 12. Dezember 1997 
  Published    1998 
  Keywords    A5-Diphosphete, l-Aza-2A5, 4A5-diphosphinine, NMR Spectra, X-Ray Data 2, 2, 4, 4-Tetrakis 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0443.pdf 
 Identifier    ZNB-1998-53b-0443 
 Volume    53 
73Author    Andreas Böhm, Kurt Polborn, Karlheinz Sünkel, Wolfgang BeckRequires cookie*
 Title    Metallkomplexe mit biologisch wichtigen Liganden, CIV [1]. or/Zio-Palladierte Komplexe von N,N-DimethyI-C-phenyl-glycinmethylester. Synthese von a-Aminosäure-Derivaten durch Insertion von Isocyaniden, CO, Alkenen und Alkinen in die Pd-C-Bindung Metal Complexes of Biologically Important Ligands, CIV [ 1]. o/t/20-Palladated Complexes of N,N-Dimethyl-C-phenylglycine-methylester. Synthesis of ct-Amino Acid Derivatives by Insertion of Isocyanides, CO, Alkenes, and Alkynes into the Pd-C Bond  
 Abstract    -phenylglycinemethylester reacts with Pd(OAc)2 in acetic acid to give the orthopalladated, acetato bridged complex 1. Treatment of 1 with sodium halide affords the chlo-ro, bromo, and iodo bridged compounds [Me2N C (H)(C 02Me)C6H4PdX]2 (2a -c) (X = halide). From 2a and 1,1 '-bis(diphenylphosphino)ferrocene the phosphine bridged trinuclear complex 3 is obtained. Substitution of the amine ligand of 2a by the phosphino group is observed for the reaction of 2a with Ph2PC(Me)C(Me)PPh2. Insertion of 2,6-dimethyl-phenylisocyanide, CO, alkyl-vinyl-ketones, and diphenylacetylene into the Pd-C bond o f 2a -c provides the ortho­ substituted organic and organometallic derivatives of phenylglycine 6a -c, 7, 8a -b and 9a -c. The crystal structures of 1, 4a, 6a, 7 and 9a were determined by X-ray diffraction. 
  Reference    Z. Naturforsch. 53b, 448—458 (1998); eingegangen am 19. Dezember 1997 
  Published    1998 
  Keywords    Palladium(II) Complexes, ortho-Palladation, N, N-Dimethyl-C-phenylglycine, Insertion Reactions N, N-Dimethyl-C 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0448.pdf 
 Identifier    ZNB-1998-53b-0448 
 Volume    53 
74Author    Wilfried Knott, Georg Frommeyerb, AstridK. Lapdor1, Dagmar WindbielaRequires cookie*
 Title    Neue Synthesen mit Magnesiumhydrid. Teil 3: Herstellung nanokristalliner und amorpher Metalle durch Hydridreduktion New Syntheses with Magnesium Hydride. Part 3: Preparation of Nanocrystalline or Amorphous Metals by Hydride Reduction  
 Abstract    The tribochemical reduction of metal halides by magnesium hydride in organic solvents allows the synthesis of nanosize or amorphous metals. 
  Reference    Z. Naturforsch. 53b, 459—468 (1998); eingegangen am 1. Dezember 1997 
  Published    1998 
  Keywords    Nanocrystalline Metals, Amorphous Metals, Hydride Reduction, Magnesium Hydride 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0459.pdf 
 Identifier    ZNB-1998-53b-0459 
 Volume    53 
75Author    Kazuhiko Ozutsumi3, Shintaro Ohnishia, Hitoshi Ohtaki, Masaaki TabatabRequires cookie*
 Title    Structure of the Short-Lived Intermediate Formed during the Metal Substitution Reaction of the Mercury(II) Porphyrin Complex with Cobalt(II) Ion in Aqueous Solution Determined by the Stopped-Flow EXAFS Method Structure of Short-Lived Intermediate, Stopped-Flow EXAFS, Metal Substitution Reaction, Cobalt(II) Porphyrin Complexes, Cobalt(III) Porphyrin Complex  
  Reference    Z. Naturforsch. 53b, 469—475 (1998); received November 20 1997 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0469.pdf 
 Identifier    ZNB-1998-53b-0469 
 Volume    53 
76Author    Henri Brunner, Bernd HaßlerRequires cookie*
 Title    Enantioselective Catalysis, 120 [1] New Optically Active Pyrrole-oxazolines  
 Abstract    14 new optically active pyrrole-oxazolines were synthesised from 2-pyrrole-carbonitrile or methyl 2-pyrrole-carboximidate and chiral amino alcohols. Their use in copper-catalysed enan­ tioselective cyclopropanation reactions gave only low optical yields (3-14%ee). 
  Reference    Z. Naturforsch. 53b, 476—480 (1998); received January 12 1998 
  Published    1998 
  Keywords    Pyrrole-oxazolines, Enantioselectivity, Catalysis, Cyclopropanations 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0476.pdf 
 Identifier    ZNB-1998-53b-0476 
 Volume    53 
77Author    VladimirA. Ovchynnikov3, VladimirM. Amirkhanov3 ', TarasP. Timoshenko3, Tadeusz Glowiakb, Henryk KozlowskibRequires cookie*
 Title    Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide  
 Abstract    Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(0)NHP(0)[N(CH2CH2)2 0 ] 2 [HL] and its sodium [NaL] and morpholine [HN(CH2CH2) 2 0 HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) A, b = 16.056(3) A, c = 9.622(2) Ä, ß = 108.55(3)°, space group P2i/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups. 
  Reference    Z. Naturforsch. 53b, 481—484 (1998); received November 11 1997 
  Published    1998 
  Keywords    Carbacylamidophosphates, IR Data, X-Ray Data 
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 Identifier    ZNB-1998-53b-0481 
 Volume    53 
78Author    Requires cookie*
 Title    Absolute Configuration of Chiral l,3>4,5-Tetrahydro-2//-l,5-benzodiazepin-2-ones  
  Reference    Z. Naturforsch. 53b, 485 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0485 
 Volume    53 
79Author    A., H. El, M. Aleem, Hussein OstafaRequires cookie*
 Title    Utility of Cyano Acid Hydrazide in Heterocyclic Chemistry: A New Route for the Synthesis of New l,2,4-Triazolo[l,5-a]pyridines and l,2,4-Triazolo[l,5-a]isoquinolines  
  Reference    Z. Naturforsch. 53b, 488 (1998) 
  Published    1998 
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 Identifier    ZNB-1998-53b-0488 
 Volume    53 
80Author    Requires cookie*
 Title    CT Complexes Derived from Verdazyl Radicals  
 Abstract    Shin'ichi N akatsuji3 *, A k ari K itam u ra3, A tsushi T akai3 Kazuyoshi N ishikaw ab, Yukio M o rim o to b, N o ritaki Y asuokab, H aru k i K aw am ura,3 H iroyuki A nzai3 
  Reference    Z. Naturforsch. 53b, 495 (1998) 
  Published    1998 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0495.pdf 
 Identifier    ZNB-1998-53b-0495 
 Volume    53 
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