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2001 (200)
61Author    AlexanderV. Shtemenko3, AlexanderA. Golichenko3, KonstantinV. DomasevitchbRequires cookie*
 Title    Synthesis of Novel Tetracarboxylato Dirhenium(III) Compounds and Crystal Structure of [Re2 (l-Adamantylcarboxylate)4Cl2] * 4 CHC13  
 Abstract    The coordination compounds o f the general formula Re2 (1^ 4X2 (X = Cl, Br; L = 1 -adamantyl-carboxylate and 1 -adamantylacetate) have been prepared and characterized by means of UV-VIS spectroscopy (20000 cm-1 , 6 —► 6*). The crystal and molecular structure of Re2(AdCOO)4Cl2 • 4 CHCI3 solvate was determined by X-ray diffraction. The units Re2(AdCOO)4Cl2 adopt a centrosymmetric dinuclear array with each metal atom coordinated in a distorted octahedron comprising one rhenium and one chlorine atoms (Re-Cl 2.505(2) A) and four carboxylate oxygen atoms in the equatorial plane. The rhenium-rhenium separation of 2.2300(5) A corre­ sponds to quadruple bond between the metal atoms. All R e-0 bonds have an almost uniform length (2.017(4) -2.032(4) A) and do not differ essentially from the parameters reported for related compounds. The closest environment of the Re2(AdCOO)4Cl2 molecules in the crystal comprises weak Cl— HC hydrogen bonds with the chloroform molecules and significantly shortened van der Waals contacts Cl— Cl, 3.46 A. 
  Reference    Z. Naturforsch. 56b, 381—385 (2001); received December 15 2000 
  Published    2001 
  Keywords    Rhenium, Clusters, Adamantane 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-0381.pdf 
 Identifier    ZNB-2001-56b-0381 
 Volume    56 
62Author    JohnG. Palmer, PaulA. Doemeny, GerhardN. SchrauzerRequires cookie*
 Title    The Chemical Evolution of a Nitrogenase Model, XXIII. The Nature of the Active Site and the Role of Homocitric Acid in MoFe-Nitrogenase  
 Abstract    The iron-molybdenum cofactor (FeMo-co) of bacterial nitrogenase is a heterometallic cluster of composition MoFe7S9 that is attached to the apoprotein by a coordinative Mo-N bond to the imidazole group of hisa442, and by a Fe-S bond to cysa.215. The molybdenum atom of FeMo-co in the enzyme in addition is coordinated to one molecule of homocitrate (he), which is required for maximal N2 reducing activity. The molybdenum atom in the enzyme-bound FeMo-co thus is hexacoordinated and cannot react with substrates unless free coordination sites are made available. It is proposed that the reactions of the substrates o f nitrogenase occur at a molybdenum active site consisting of a mononuclear molybdenum homocitrate complex attached to hisaAA2 of the apoprotein that in the functional enzyme is generated from FeMo-co by a reversible, redox-linked dissociation of the Fe7S9-c;y5' cluster. Studies with catalytic model systems consisting of complexes of molybdenum with imidazole and hydroxo-carboxylate ligands support this proposal and provide a rationale for the specific activating effect of homocitrate in nitrogenase. 
  Reference    Z. Naturforsch. 56b, 386—393 (2001); received January 17 2001 
  Published    2001 
  Keywords    Nitrogen, Acetylene, Homocitric Acid 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-0386.pdf 
 Identifier    ZNB-2001-56b-0386 
 Volume    56 
63Author    SaharI. Mostafa3, SpyrosP. Perlepesb, Nick HadjiliadiscRequires cookie*
 Title    New Dinuclear Transition Metal Complexes with the [M2(//-dhbq)]n+ Core and 2-(2'-Pyridyl)quinoxaline (L) as a Terminal Ligand: Preparation and Characterization (dhbq2-= the Dianion of 2,5-Dihydroxy -1,4  
 Abstract    2,5-Dihydroxy-l,4-benzoquinonate(-2) Complexes, Dinuclear Complexes, 2-(2'-Pyridyl)quinoxaline Complexes Synthetic procedures are described that allow access to the new complexes [Mn2(dhbq)L2(H20) 4 (1), [F e^dM xO M ^O ^K N C ^V öIL O (2), [Co2(dhbq)Cl2L2(H20) 2] (3), [Ni2(dhbq)Cl2L2(H20) 2] (4), [Cu2(dhbq)Cl2L2(H20) 2] (5), [Ru2(dhbq)L2(H20)4](C104)2 (6), [Rh2(dhbq)Cl2L2(H20) 2]Cl2-2H20 (7), [Pd2(dhbq)L2]Cl2-5H20 (8) and [A g^dhbq)^] (9), where dhbq2-is the dianion of 2,5-dihydroxy-1,4-benzoquinone and L is the biheteroar-omatic ligand 2-(2'-pyridyl)quinoxaline. The new complexes were characterized by elemental analyses and by a variety of physical and spectroscopic techniques. Dinuclear structures are assigned for the complexes in the solid state. The two metal ions are bridged by the bis-chelating dhbq2-ion, while L behaves as a bidentate chelate with the 2'-pyridyl nitrogen and the nearest quinoxaline nitrogen atom as the ligand atoms. The metal ion coordination geometries are octahedral, tetrahedral or square planar. 
  Reference    Z. Naturforsch. 56b, 394—402 (2001); received December 28 2000 
  Published    2001 
  Keywords    benzoquinone, M = Ag1, Mn11, Co11, Ni", Cu11, Ru11, Pd11, Fem, Rhm, n = 0, 2, 4) 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-0394.pdf 
 Identifier    ZNB-2001-56b-0394 
 Volume    56 
64Author    W. Olfgang BeckRequires cookie*
 Title    Metallkomplexe mit biologisch wichtigen Liganden, CXXXVII [1]. Halbsandwich-Komplexe mit N, O-Chelaten und Schiff-Basen von /?-Aminosäuren  
 Abstract    M etal C om plexes o f Biologically Im p o rta n t Ligands, C X X X V II [1]. Halfsandw ich C om plexes w ith A^O -Chelates and Schiff Bases of ß -A m ino Acids D aniela Koch, W infried H offm üller, K urt Polborn ß-Alanine, /3-Phenylalanine, Ruthenium /2-Phenylalanine forms with chloro bridged complexes the chiral /V,0-chelates Cp*Ir(Cl)(NH2CH(Ph)CH2C 0 2) and (p-cymene)Ru(Cl)(NH2CHPhCH2C 0 2) as mixture of two diastereoisomers. Similarly the palladium(III) and platinum(II) complexes (Et3P)(Cl)M(NH-.CH(Ph)CH2CO'.) (M = Pd, Pt) were obtained. Schiff base complexes (arene)(Cl)M (02CC(R)=N-CH(R)CH(R)CH2C 0 2CH3) (arene = Cp*, p-cymene; M = Ir, Ru) were synthesized from the chloro-bridged compounds, 2-oxocarboxylates and yS-alanine or ^-phenylalanine methylester. The Cp*Ir complex with a tridendate dianionic Schiff base generated from pyruvate and /3-phenylalaninate is obtained as a single isomer. Cp*Ir(Cl) forms a complex with an 7V,0-bidentate Schiff base ligand from glycinate and acetylacetic ethyl ester. 
  Reference    Z. Naturforsch. 56b, 403—410 (2001); eingegangen am 26. Februar 2001 
  Published    2001 
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 Identifier    ZNB-2001-56b-0403 
 Volume    56 
65Author    Z. NaturforschRequires cookie*
 Title    Synthesis of «-Tocopheryl Glycosides  
 Abstract    An unusual course of d-a-tocopherol glucosylation by the Helferich method was observed. The product distribution very depended on acid catalyst and solvent used. The /?-glucoside was accompanied by an unsaturated a-glucoside. Other unsaturated d-a-tocopheryl gluco-sides were obtained by reactions with acetylated glucal and 2-acetoxy glucal. 
  Reference    Z. Naturforsch. 56b, 411 (2001); received April 10 2000 
  Published    2001 
  Keywords    Vitamin E, Glucosylation, a-Tocopheryl Glycosides 
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 TEI-XML for    default:Reihe_B/56/ZNB-2001-56b-0411.pdf 
 Identifier    ZNB-2001-56b-0411 
 Volume    56 
66Author    K. Rystyna Bogdanowicz-Szwed, A. Leksandra, P. AłaszRequires cookie*
 Title    Synthesis of 3,4-Dihydro-2/f-pyrans by Hetero-Diels-Alder Reactions of Functionalized a,/?-Unsaturated Carbonyl Compounds with Styrenes  
 Abstract    H etero-D iels-A lder Reaction, a,/?-Unsaturated Ketones, Styrenes Cycloadditions of 3-aryl-2-benzoyl-2-propenenitriles la,b to styrene (2a) and its methyl-or methoxy-substituted derivatives 2b-d proceed regio-and diastereoselectively yielding cis and trans diastereoisomers of 2,4,6-triaryl-3,4-dihydro-2//-pyran-5-carbonitriles 3 and 4 in 59-72% yield. Cycloadducts cis-3 were the major products. Reaction of 5-(4-nitrobenzyli-dene)-l,3-dimethylbarbituric acid (5) with styrenes 2a-d afforded diastereoisomeric mixtures of 2//-pyrano[2,3-d]pyrim idine-2,4(3//)-diones cis-6 
  Reference    Z. Naturforsch. 56b, 416 (2001); received D ecem ber 12 2000 
  Published    2001 
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 Identifier    ZNB-2001-56b-0416 
 Volume    56 
67Author    C. H. Och, C. R.Requires cookie*
 Title    Alkalimetall-Oxosilicate A6[Si30 9] und A 6[Si20 7] (A = Rb, Cs): Darstellung und Kristallstruktur  
 Abstract    The A lkaline M etal O xo-Silicates A 6[Si30 9] and A 6[Si20 7] (A = Rb, Cs): P rep aratio n and Crystal Structure The title compounds were synthesized via reaction of quartz and A 0 2 (A = Rb, Cs) with the elem ental alkali metals. Their crystal structures were determ ined on the basis o f single crystal X-ray data. A ll compounds crystallize in the m onoclinic system with space group P2j/c and lattice constants a = 656.0(l)/684.7(3), b = 1329.7(3)/1375.7(4), c = 1647.6(3)/1703.6(8) pm, ß = 107.78(3)/108.23(2)°, Z = 4 (A 6[Si30 9], A = Rb/Cs) and a = 668.59(8)/711.4(1), b = 911.37(9)/952.1(2), c = 1121.09(9)/1192.7(7) pm, ß = 125.52(9)/126.22(3)°, Z = 2 (A 6[Si20 7], A = Rb/Cs) respectively. The rubidium and cesium compounds are isotypic with the corre­ sponding potassium silicates. 
  Reference    Z. Naturforsch. 56b, 423 (2001); eingegangen am 8. Februar 2001 
  Published    2001 
  Keywords    Silicates, Disilicates, Cyclotrisilicates 
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 Identifier    ZNB-2001-56b-0423 
 Volume    56 
68Author    H. O. Rst, K. Unkely, A. Rn, D. VoglerRequires cookie*
 Title    Optical Outer-Sphere Charge Transfer and Photoreactivity of the Ion Pair Tetrabutylammonium Tetrabutylborate  
 Abstract    Photochemistry, Tetraalkylammonium, Tetraalkylborate The ion pair [N(n-butyl)4]+[B(n-butyl)4]~ in CC14 shows a BR 4" — » N R 4+ outer-sphere charge transfer (OSCT) absorption at X = 306 nm (sh, e = 420 dm3 M -1 cm -1). OSCT excitation of the ion pair in CH2C12 (Airr > 275 nm) leads to a photo­ lysis with (p = 1.5 x 10~3 at Airr = 280 nm. Octane is formed as photoproduct. 
  Reference    Z. Naturforsch. 56b, 431 (2001); received February 12 2001 
  Published    2001 
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 Identifier    ZNB-2001-56b-0431_n 
 Volume    56 
69Author    M. Artin JansenRequires cookie*
 Title    Rb8A 104Au3 = Rb5A 104 * 3RbAu - ein Aluminat-Aurid  
 Abstract    R b 8A 1 0 4A u3 = R b 5A 1 0 4-3RbAu -an A lu m in ate A uride A nja-V eren a M udring R b8A 1 0 4Au3 (Pearson-Code oP64, /*212121, a = 1043.4(1), b = 1296.7(2), c = 1320.2(2) pm, Z = 4, 809 reflections with IQ > 2a(I), Rj = 0.059, w R 2 = 0.151) is a further, completely new representative belonging to the group of composite alkali metal aurides. It consists of structural elem ents of alkali orthoaluminates and alkali aurides. Indeed, Rb8A 1 0 4Au3 is thus better represented by the formula Rb5A 1 0 4-3RbAu. 
  Reference    Z. Naturforsch. 56b, 433—4 (2001); eingegangen am 14. Februar 2001 
  Published    2001 
  Keywords    Alum inates, Aurides, Solid State Synthesis 
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 Identifier    ZNB-2001-56b-0433_n 
 Volume    56 
70Author    M. Arco, H. Klingele, B. Erth, Ld KerstingRequires cookie*
 Title    E fficient M edium -Scale Synthesis o f 2-Brom o-5-te/-f-butylbenzene- 1,3-dicarbaldehyde  
 Abstract    2-Bromo-5-rert-butylbenzene-l,3-dicarbaldehyde, B enzene Derivatives A short and efficient multi-gram synthesis of the title compound has been designed which al­ lows its preparation from commercially available material in only three steps in overall yields of 6 0 -7 0 % . 
  Reference    Z. Naturforsch. 56b, 437 (2001); received D ecem ber 27 2000 
  Published    2001 
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 Identifier    ZNB-2001-56b-0437_n 
 Volume    56 
71Author    Rb Ert, W. M. Itzel, C. Hristian, Lustig, Sandra ScharfeRequires cookie*
 Title    C ocrystallisation o f Trim ethylchloro- stannane with a D istan n oxane  
 Abstract    Tin, Stannoxanes, Supramolecular Aggregate Partial hydrolysis of a mixture o f M e2SnCl2 and M e3SnCl affords an aggregate of the composition [Sn2C l(0)(0 S n M e 3)(M e)4]2 which cocrystallises with two equivalents of M e3SnCl to form endless bands of {[Sn2C l(0)(0 S n M e 3)(M e)4]2-2M e3SnCl}x linked through Sn • • • Cl intermolecu-lar contacts. 
  Reference    Z. Naturforsch. 56b, 440 (2001); received March 2 2001 
  Published    2001 
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 Identifier    ZNB-2001-56b-0440_n 
 Volume    56 
72Author    N. O. Rb, E. Rt, W. M. Itzel, Christian LustigRequires cookie*
 Title    Crystal Structure of a Lithium Chloride Cubane Cluster Solvated by Diethyl Ether  
  Reference    Z. Naturforsch. 56b, 443 (2001); received March 2 2001 
  Published    2001 
  Keywords    Lithium Chloride, Aggregation, Crystal Structure 
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 Identifier    ZNB-2001-56b-0443_n 
 Volume    56 
73Author    Requires cookie*
 Title    Synthesis and Structure o f Y bP dSn2  
 Abstract    D irk Kußm ann and R ainer P öttgen D ep artm en t C h em ie, Ludw ig-M axim ilians-U n iversität M ünchen, B utenan dtstraß e 5 -1 3 (H aus D), D -81377 M ünchen, G erm any 
  Reference    Z. Naturforsch. 56b, 446 (2001) 
  Published    2001 
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 Identifier    ZNB-2001-56b-0446_n 
 Volume    56 
74Author    Requires cookie*
 Title    D eoxycyclop ald ic A cid and C yclopaldic  
 Abstract    A cid , Plant Growth R egulators, P roduced by P e n ic illiu m sp. 
  Reference    Z. Naturforsch. 56b, 449 (2001) 
  Published    2001 
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 Identifier    ZNB-2001-56b-0449_n 
 Volume    56 
75Author    Johannes Beck, Alexander StankowskiRequires cookie*
 Title    A One-Dimensional Polymeric Form of the Polycation Te82+ in the Structure of Te8[Bi4Cl14]  
 Abstract    catena-Octatellurium(2+), Main Group Element Clusters, Chalcogen Polycations The reaction of Te, TeCl4 and BiC^ in a sealed evacuated glass ampoule in a temperature gradient 160 to 90 °C yields Te8[Bi4Cli4] as black platelike crystals with a golden lustre which are deposited in the temperature zone 150 to 130 °C. The best yield is obtained with a Te/TeCU/BiCls molar ratio of 15/3/4. The crystal structure determination (orthorhombic, P 2 i2 ,2 i, a = 879.9(3), b = 1642.3(4), c = 2267.3(8) pm, Z = 4) shows that Te8[Bi4Cl14] consists o f a novel one-dimensional (Te82+)" polycation and a two-dimensional chlorobismutate anion Bi4Cli42_. The structure of the cation consists of boat shaped Te6 rings which are connected in the 1,4-positions by Te2 groups to a one-dimensional polymeric strand. The structure is substantially different from the previously reported Teg2+ polycations in TegtWCUh and TegtMClö] (M = Zr, Hf, Re) where discrete bicyclic clusters with only weak interionic interactions are present. The Bi4Cli42_ ion can be described as built up of BiCb molecules which are connected by Cl~ ions to a two-dimensional network [(BiCl3)4(Cl-)2]". 
  Reference    Z. Naturforsch. 56b, 453—457 (2001); received March 9 2001 
  Published    2001 
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 Identifier    ZNB-2001-56b-0453 
 Volume    56 
76Author    EvaS. Schm, A. Nnette Schier, NorbertW M Itzel, Hubert SchmidbaurRequires cookie*
 Title    Preparation and Structure of Cyclic Gallium(III) and Gallium(II) 2-Amino-ethyl-amides  
 Abstract    Gallium(III) and Gallium(II) Amides, Gallium Amino Complexes, Gallium Coordination The reaction of /V,/V-di('butyl)-ethane-1,2-diamine with NaH followed by anhydrous GaCl3 (molar ratios 1:2 :1) gives mainly an insoluble bis(diamido)gallium chloride together with a low yield (28%) of a soluble monocyclic dichlorogallium-[2-('butylamino)-ethyl-('butyl)amide], ChGaCBuNH-CHaCHi-N'Bu) 1, the structure of which has been determined. Metallation of the same diamine with 'butyl-lithium and GaCb (1:2:1) gave small quantities of the corresponding dinuclear, bicyclic gallium(II) compound 2, [('BuNH-CH2CH2-N'Bu)GaCl]2 with a Ga-Ga single bond connecting the two units, as again shown by a single crystal X-ray diffraction analysis. 
  Reference    Z. Naturforsch. 56b, 458—462 (2001); received April 4 2001 
  Published    2001 
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 Identifier    ZNB-2001-56b-0458 
 Volume    56 
77Author    Ratikanta Mishra, Rainer Pöttgen, Gunter KotzybaRequires cookie*
 Title    New Metal-Rich Compounds NblrSi, NblrGe, and TalrSi -Synthesis, Structure, and Magnetic Properties  
 Abstract    The metal-rich intermetallic compounds NblrSi, NblrGe, and TalrSi were synthesized by arc-melting of the elements and subsequent annealing in glassy carbon crucibles in a high-fre-quency furnace. The three compounds were investigated by X-ray diffraction on powders and single crystals: TiNiSi type, Pnma, a = 641.27(3), b = 379.48(2), c = 727.70(3) pm, wR2 = 0.0773, 430 F 2 values for NblrSi, a = 645.48(3), b = 389.21(2), c = 741.11(4) pm, wR2 = 0.0981, 297 F 2 values for NblrGe, and a = 638.11(3), b = 378.69(2), c = 726.78(3) pm, wR2 = 0.0887, 290 F 2 values for TalrSi with 20 variables for each refinement. The iridium and silicon (germanium) atoms form a three-dimensional network of puckered IrjSi3 and Ir3Ge3 hexagons in which the niobium (tantalum) atoms fill larger cages. Magnetic susceptibility measurements on NblrSi and TalrSi indicate Pauli paramagnetism with room temperature susceptibilities of 0.30(5)-10~9 and 0.97(5)-10-9 m3/mol, respectively. 
  Reference    Z. Naturforsch. 56b, 463 (2001); received April 30 2001 
  Published    2001 
  Keywords    Silicides, Germanides, Magnetic Properties 
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 Identifier    ZNB-2001-56b-0463 
 Volume    56 
78Author    HansB. Ock, ErikH. EigelRequires cookie*
 Title    Interaction in M olecular Crystals, 174 [1, 2]. Crystal Growth and Structure D eterm ination o f D ifferently M ethyl-Substituted Tetraphenyl Im idodiphosphates  
 Abstract    Four differently methyl-substituted tetraphenyl imidodiphosphates [(H3C)nC6H5_ J 2PO-NH-PO[C6H5_n(CH3)n] (n = 1, 2), i. e. the 4-, 3,4-, 3,5-and 2,3-derivatives, have been crystal­ lized and their structures determined to gain information on the spatial requirements as ligands in the corresponding cesium salts. According to the packing coefficients calculated from the structural data, they increase in the sequence 4 < 3,5 < 3,4 < 2,3. The most perturbed structural motif is the hydrogen bonded, eight-membered ring of each the dimer subunits. 
  Reference    Z. Naturforsch. 56b, 469—182 (2001); eingegangen am 21. Dezember 2000 
  Published    2001 
  Keywords    Imidodiphosphate Methyl-Substituted Tetraphenyl Esters, Spatial Overcrowding, Structure Correlation 
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 Identifier    ZNB-2001-56b-0469 
 Volume    56 
79Author    Hans Bock, Erik Heigel, Zdenek Havlas3Requires cookie*
 Title    Wechselwirkungen in Molekülkristallen, 175 [1, 2]. Kristallzüchtung und Strukturbestimmung von {Cäsium-tetraphenylimido- diphosphatj-Aggregaten mit unterschiedlicher lipophiler Umhüllung durch verschiedenartig Methyl-substituierte Phenylringe sowie relativistische DFT-Modellberechnungen zu Cäsium/Cäsium-Wechselwirkungen Interaction in M olecular Crystals, 175 [1,2]. Crystal Growth and Structure Determination of {Cesium-tetraphenylimidodiphosphate} Aggregates with Differing Lipophilic Wrapping Due to Differently Methyl-Substituted Phenyl Rings, and Relativistic DFT-Model Calculations of Cesium/Cesium Interactions  
 Abstract    In alkali-tetraphenylimidodiphosphate ion aggregates, the size of the cation determines the curvature of the ligand and, therefore, whether hexameric ellipsoidal clusters or polymeric chains are formed. To further characterize the ligand spatial requirements, the phenyl rings have been methylsubstituted in 4-, 3/5-, 3/4-or 2,3-positions, their conformations structurally analyzed and correlated with the van der Waals substituent profiles. In addition, relativistic density functional theory potential curves have been calculated for the Cs0 --Cs® interactions in simplified model systems. 
  Reference    Z. Naturforsch. 56b, 483—511 (2001); eingegangen am 21. Dezember 2000 
  Published    2001 
  Keywords    Cesium Tetraphenylimidodiphosphates, Methyl Substitution Effects, Polyion Aggregates, Crystal Structures 
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 Identifier    ZNB-2001-56b-0483 
 Volume    56 
80Author    Comet Gmbh, Pyrotechnik ApparatebauRequires cookie*
 Title    Fluoreliminierung aus Graphitfluorid mit Magnesium Defluorination of Graphite Fluoride Applying Magnesium Emst-Christian Koch  
 Abstract    Consolidated stoichiometric mixtures of graphite fluoride (1) and magnesium (2) upon igni­ tion under argon atmosphere (0,1 MPa) yield very high flame temperature of ~ 5600 K as determined by infrared emission spectroscopy. The combustion product was analysed by X-ray powder diffraction and revealed the presence of magnesium fluoride and graphite as well as structurally low ordered carbon. A possible reaction mechanism is discussed. 
  Reference    Z. Naturforsch. 56b, 512—516 (2001); eingegangen am 5. März 2001 
  Published    2001 
  Keywords    Graphite Fluoride, Defluorination, Magnesium 
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 Identifier    ZNB-2001-56b-0512 
 Volume    56 
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