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1996[X]
101Author    KhalidM. Ohammed Khana, Farnaz Malikb, Mashooda Hasanb, Shahnaz Perveen3, Jodwiga Frelekc, G. Ünther Snatzke+, Wolfgang Voelter3Requires cookie*
 Title    Circular Dichroism Studies on New Optically Active 1,5-Benzodiazepine Derivatives  
 Abstract    From thirty three new optically active 1,5-benzodiazepine derivatives the UV and CD data are reported and the bands discussed related to corresponding electronic transitions respectively stereochemical features. 
  Reference    Z. Naturforsch. 51b, 588—598 (1996); recieved September 26 1995 
  Published    1996 
  Keywords    CD Spectra, Benzodiazepines, Chiral 1, 5-Benzodiazepine Derivatives 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0588.pdf 
 Identifier    ZNB-1996-51b-0588 
 Volume    51 
102Author    Rolf Minkwitz, RaimUnd Bröchler, Hans PreutRequires cookie*
 Title    Low-Temperature Crystal Structure of the Inclusion Compound {[N(CH3)4+C1]2] * CH 3CN * h 2o  
 Abstract    The crystal structure of {[N(CH3)4+C1]2}-CFI3C N H 20 is reported. Cry-stalls are orthorhombic, space group Pnma, with a = 1622.9(15), b = 671.3(6), c = 1511.2(11) pm, V = 1646(2) 106 pm3 and Z = 4. 
  Reference    Z. Naturforsch. 51b, 599—601 (1996); eingegangen am 3. August 1995 
  Published    1996 
  Keywords    Preparation, Crystal Structure, Inclusion Compound 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0599_n.pdf 
 Identifier    ZNB-1996-51b-0599_n 
 Volume    51 
103Author    Bernhard Neumüller, Felora Heshm, Kurt DehnickeRequires cookie*
 Title    Crystal Structure of [(THF)2Li(/*2-Cl)2TiCl?(THF)2]  
 Abstract    The crystal structure of the title com pound has been determined by X-ray methods. Space group C2/c, Z = 4, lattice dimensions at -8 0 °C: a = 1343.8(2), b = 1031.6(1), c = 1669.4(1) pm, ß = 96.47(1)°. The compound forms an ion pair in which the lithium atom is coordinated in a distorted tetrahedral geometry by two T H F mole­ cules and by two chlorine atoms. The halide atoms have a /^-bridging function, coordinating the li­ thium and the titanium center. The titanium atom possesses a distorted octahedral environm ent with two TH F ligands in rrans-position. 
  Reference    Z. Naturforsch. 51b, 602—604 (1996); eingegangen am 23. O ktober 1995 
  Published    1996 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0602_n.pdf 
 Identifier    ZNB-1996-51b-0602_n 
 Volume    51 
104Author    Karsten Fischer, Elisabeth Feldbaum-M, Petra Öller, Volker Vogt, Horst Winter, SabrowskyRequires cookie*
 Title    CsNaTe -D arstellung und Charakterisierung von Cäsium natrium tellurid CsNaTe -Preparation and Characterization of Cesium Sodium Telluride  
 Abstract    X-Ray, Cesium Sodium Telluride The dark green compound CsNaTe has been prepared. The characterization by X-ray powder methods leads to a tetragonal lattice (P4/nmm) with a = 530.8 (4), c = 853.2 (1) pm and Z = 2. The structure ist related to the PbFCl structure type. 
  Reference    Z. Naturforsch. 51b, 605—606 (1996); eingegangen am 18. Januar 1995 
  Published    1996 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0605_n.pdf 
 Identifier    ZNB-1996-51b-0605_n 
 Volume    51 
105Author    Claus Feldm, M. Artin, Jansen5Requires cookie*
 Title    O ptische A b sorp tion der A uride M3A11O ( Optical Absorption of the Aurides M3AuO (M = K, Rb, Cs)  
 Abstract    The optical absorption of the aurides M3AuO (M = K, Rb, Cs) and CsAu has been determ inated by UV/VIS spectroscopy. The band gaps have been found to be 2,35(2) eV (Cs3AuO) and 2,30(2) eV (CsAu). This corresponds to a more pronounced anionic character of gold in Cs3AuO as com pared to CsAu. In the case of K3AuO and R b3AuO no band gap was detectable. 
  Reference    Z. Naturforsch. 51b, 607—608 (1996); eingegangen am 24. Juli 1995 
  Published    1996 
  Keywords    Aurides, Optical A bsorption, UV-VIS Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0607_n.pdf 
 Identifier    ZNB-1996-51b-0607_n 
 Volume    51 
106Author    D. Bublitz, A. Franken, W. Preetz, H. ThomsenRequires cookie*
 Title    Darstellung, U B-NMR-Spektren, Schwingungsspektren und Normalkoordi- natenanalyse von cowy'HWcto-Bis-hexahydro-c/oso-hexaborat, [B6H6-B 6H6]2_, sowie Kristallstruktur von [P(C6H5)4 ]2-cöW7 ww^o-[B6H6-B 6H6 ] Preparation, 11B NMR Spectra, Vibrational Spectra and Normal Coordinate Analysis of con ju ncto-B is-h exah ydro-closo-h exaboratQ , [B6H6-B 6H6]2_, and the Crystal Structure of [ P(C6 H5 )4 ] 2 -conjuncto-[B6 H6-B 6 H6 ]  
 Abstract    By reaction of [B6H6]2-with dibenzoylperoxide in dichloromethane conjuncto-[B6H6-b 6h 6]2-is formed. The product could be separated from excess [B6H6]2 by ion exchange chro­ matography on diethylaminoethyl cellulose. The crystal structure of [P(C6H^ ^ -con ju n cto-[B6H6-B 6H6 ] has been determined by single crystal X-ray diffraction analysis; triclinic, space group PI with a = 10.8315(10), b = 11,2422(12), c = 20.340(2) Ä, a = 91.278° (9), ß = 9 0 .\78° (9), 7 = 105.662°(9). The 1 'B NMR spectrum reveals three signals with the intensity ratio 1:1:4, for two equivalent moieties of the conjuncto molecule ion with local C4v symmetry. The IR and Raman spectra of the deprotonated Cs salts of the 1()B, n B and their respective D isotopomers of conjuncto-[B6H5-B6HS]4_ exhibit characteristic shifts. Using averaged crystallographic data and assuming idealized D4h symmetry, normal coordinate analyses have been performed based on a modified valence force field. With a set of eleven force constants (e.g. fd(BB)C 0njU IK.t0 = 2.9, fd(BB)cage = 1.6 mdyn/A) very good agreement between observed and calculated frequencies has been achieved. From strong vibrational coupling with the B6 clusters two vibrations result for the conjuncto B-B bond at 1142/1198 and 292/304cm-1 for 1 'B/I(IB species, respectively. They can be assigned as anti-phase and in-phase motions of the conjuncto B atoms related to the equatorial B4 planes. 
  Reference    Z. Naturforsch. 51b, 609—618 (1996); eingegangen am 7. September 1995 
  Published    1996 
  Keywords    Crystal Structure, n B NMR Spectra, Vibra­ tional Spectra, Normal Coordinate Analysis 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0609_n.pdf 
 Identifier    ZNB-1996-51b-0609_n 
 Volume    51 
107Author    KarinD. Öllinga, Andre Krugb, Helmut Hartungb, Horst WeichmannaRequires cookie*
 Title    Reaktion von Iodomethylzinnverbindungen mit (S)-l-f-Butyloxycarbonyl- 2-f-butyl-3-methyl-4-imidazolidinon (Boc-BMI) Reaction o f Iodomethyltin Compounds with (S^-l-r-Butyloxycarbonyl- 2-?-butyl-3-methyl-4-imidazolidinone (Boc-BM I)  
 Abstract    Imidazolidin-4-one, Triorganostannylmethylation, 1,2-Oxastannolane Diastereoselective alkylation of (5')-2-r-butyl-l-r-butyloxycarbonyl-3-methyl-4-imidazoli-dinone (Boc-BMI) 1 with R3SnCH2I yields triorganostannylmethylated Boc-BMI compounds, 2 and 3 (2: R = Me; 3: R = Ph). By halogenation 2 and 3 are transformed into the halostannyl-substituted compounds R3_ nX"SnCH2-Boc-BMI 4 -8 (R = Me, Ph; n = 1, 2; X = Cl, Br). Analogously, the trifluoroacetyloxostannylated compounds 9 and 10 (9: R = Me; 10: R = Ph) are formed by reaction of 2 and 3 with trifluoracetic acid. 4 (R = Me; n = 1; X = Cl) has been structurally characterized in detail by NMR spectroscopy and X-ray analysis. Its tin atom is pentacoordinated by intramolecular coordination of the CO group of the imidazolidinone ring. The alkylation of 1 with Me2Sn(CH2I)2 yields the bis-Boc-BMI tin compound 11 and the iodomethyl dimethylstannylmethylated Boc-BMI 12. 11 reacts with one or two equivalents of bromine to give the bromostannylated derivatives 13 and 14, respectively. 
  Reference    Z. Naturforsch. 51b, 619—628 (1996); eingegangen am 8. November 1995 
  Published    1996 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0619.pdf 
 Identifier    ZNB-1996-51b-0619 
 Volume    51 
108Author    Nils Wiberg, Susanne WagnerRequires cookie*
 Title    Zur Reaktivität des Silaethens M e2Si=C(SiM e3 )2 : Regioselektivität, Stereo­ selektivität und relative Geschwindigkeiten von En-Reaktionen [1] On the Reactivity o f Silaethene Me2Si=C (SiM e3)2: Regioselectivity, Stereoselectivity and Relative Rates o f Ene Reactions [1]  
 Abstract    Silaethene, Ene Reactions with Propene and Derivatives, Relative Rates of Ene Reactions Ene reactions of Me2Si=C(SiMe3)2 (1) w'th propene or with methyl derivatives of propene and 1,3-butadiene, respectively, of the formula R'CH=CR2-CH2R3 take place regioselectively, as well as stereoselectively and are retarded by increasing bulk of R1, R3 (for example H < CH3 < CH=CH2 < CH=CHMe), as well as accelerated by an increasing tendency of R2 to donate electrons (for example H < CH3 « CH=CH2 < CH2SiMe2[CH(SiMe3)2]). It is concluded from these studies, that ene reactions of 1 occur concerted and are HOMOene-LUMOenophjie controlled. 
  Reference    Z. Naturforsch. 51b, 629—636 (1996); eingegangen am 8. November 1995 
  Published    1996 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0629.pdf 
 Identifier    ZNB-1996-51b-0629 
 Volume    51 
109Author    Thomas Kräuter, Bert Werner, Bernhard NeumüllerRequires cookie*
 Title    Synthese  
 Abstract    und Eigenschaften von Benzylgallium(indium)-Verbindungen. Die Kristallstrukturen von [(PhCH2)2GaBr]2, [(PhCH2)2GaN(H)f-Bu]2 und [PhCH2InCl2(THF)2] Synthesis and Properties o f Benzylgallium(indium) Compounds. The Crystal Structures o f [(PhCH2)2GaBr]2, [(PhCH2)2GaN(H)r-Bu]2 and [PhCH2InCl2(THF)2] (PhCH2)2GaBr (1) can be obtained by the redistribution reaction of GaBr3 with Ga(CH2Ph)3 in a molar ratio 1:2. Treatment of 1 or (PhCH2)2GaCl with one equivalent of LiN(H)/-Bu gives the diorganogallium amide [(PhCH2)2GaN(H)r-Bu]2 (2). The toluene-insoluble PhCH2InCl2 can be structurally investigated after dissolving in THF and crystallization as [PhCH2InCl2(THF)2] (3). 1 -3 were characterized with NMR, IR and MS techniques as well as by X-ray structure determinations. 1 forms two crystallographic independent dimers while 2 is a centrosymmetric dimer in the solid state. 3 is a monomer with a trigonal-bipyramidal coordination sphere at the indium center. 
  Reference    Z. Naturforsch. 51b, 637—645 (1996); eingegangen am 14. September 1995 
  Published    1996 
  Keywords    Gallium Compounds, Indium Compound, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0637.pdf 
 Identifier    ZNB-1996-51b-0637 
 Volume    51 
110Author    Ralf Czekalla, Wolfgang Jeitschko, Rolf-Dieter Hoffmann, Helmut RabeneckRequires cookie*
 Title    Preparation, Crystal Structure, and Properties of the Lanthanoid Carbides Ln4C7 with Ln = Ho, Er, Tm, and Lu  
 Abstract    The isotypic carbides Ln4C7 (Ln = Ho, Er, Tm, Lu) were prepared by arc-melting of the elemental components, followed by annealing at 1300 °C. The positions of the metal and of some carbon atoms of the monoclinic crystal structure of LU4C7 were determined from X-ray powder data, and the last carbon positions were found and refined from neutron powder diffraction data: P2,/c, a = 360.4(1), b = 1351.4(3), c = 629.0(2) pm, ß = 104.97(2)°, Z = 2, R = 0.026 for 429 structure factors and 15 positional parameters. The structure contains isolated carbon atoms with octahedral lutetium coordination and linear Cvunits, with C-C bond lengths of 132(1) and 135(1) pm. This carbide may therefore be considered as derived from methane and propadiene. The hydrolysis of LU4C7 with distilled water yields mainly methane and propine, while the hydrolyses of the corresponding holmium and erbium carbides resulted in relatively large amounts of saturated and unsaturated C2-hydrocarbons in addition to the expected products methane and propine. The structure comprises two-dimensionally infinite NaCl-type building elements, which are separated by the C3-units. It may be described as a stacking variant of a previously reported structure of H04C7, now designated as the a-modification. The Lu4C7-type /^-modification was obtained at higher temperatures. Its structure was refined by the Rietveld method from X-ray powder data to a residual R = 0.037 for 320 F values and 15 positional parameters. Lu4C7 is Pauli paramagnetic; /3-H04C7 and Er4C7 show Curie-Weiss behavior with magnetic ordering temperatures of less than 20 K. 
  Reference    Z. Naturforsch. 51b, 646—654 (1996); received August 28 1995 
  Published    1996 
  Keywords    Binary Lanthanoid Carbides, Magnetic Properties, Hydrolyses of Carbides, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0646.pdf 
 Identifier    ZNB-1996-51b-0646 
 Volume    51 
111Author    Dirk Johrendt, Albrecht MewisRequires cookie*
 Title    The Electronic Structure o f Ternary Transition Metal Pnictides. I. AlBo-Variants  
 Abstract    The electronic structure and bonding of some ternary AlB2-type compounds AMX (A=2a-, X=5b-element, M=transition metal) were studied by means of Extended-Hückel and TB-LMTO-ASA calculations. Previous geometric stability criteria of the AIB2 structure have been extended, and reasons for some structural peculiarities and distortions are given. A simple orbital interaction scheme based on local symmetry is used as starting point to investigate the electronic properties of these compounds, whereas the band structures of the ZrBeSi-type SrPdAs and the Peierls-distorted variants CaPdAs and BaPdP are described in more detail. The results of calculations and resistivity measurements are discussed within the scope of Zintl's concept under consideration of the transition metal d-orbitals. It turns out that these solids can be described as metallic Zintl compounds. 
  Reference    Z. Naturforsch. 51b, 655—664 (1996); eingegangen am 6. November 1995 
  Published    1996 
  Keywords    Ternary Pnictides, Electronic Structure, Stability Criteria, Zintl Concept 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0655.pdf 
 Identifier    ZNB-1996-51b-0655 
 Volume    51 
112Author    Ayhan Elmalia, Yalcin Elerman3, Ingrid Svoboda, Hartmut Fuessb, Klaus Griesar0, Wolfgang HaasecRequires cookie*
 Title    Structure and Spin-Spin Interactions in a Linear Trinuclear Ni(II) Complex  
 Abstract    [Ni3(C2H302)2(C3H8N0)2L2] 1(L=N,N'-1,3-propyl-disalicylaldimine), (C2H30 2)=acetate, (C3H><NO)=hydroxymethyl-dimethylamine] has been synthesized and its crystal structure de­ termined, [C44H54N6OioNi3], triclinic, space group Pi, a = 9.560(1), b = 10.681(1), c = 12.200(1) A ,a = 112.17(1), ß = 101.25(1), 7 = 90.32(1)°, V = 1127.3 A \ Z = l.The molecule is linearly trinuclear with octahedral coordination of each nickel ion. The Ni-Ni distance is 3.048(1) A. Each nickel(II) atom is in an octahedral coordination. Magnetic susceptibility mea­ surements in the range 4.2 < T < 280 K have revealed antiferromagnetic coupling between adjacent Ni atoms (J\ = -2.2 cm-1) and between the terminal Ni atoms (/2 = -1 .7 cm-1). 
  Reference    Z. Naturforsch. 51b, 665—670 (1996); received October 20 1994 
  Published    1996 
  Keywords    X-Ray, Linear Trinuclear Nickel Complex, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0665.pdf 
 Identifier    ZNB-1996-51b-0665 
 Volume    51 
113Author    Silke Busche, Karsten BluhmRequires cookie*
 Title    Synthese und Kristallstruktur von Lanthanoidzinkboraten L n Z n ^ O jo) mit Ln = Ce, Nd, Tb Synthesis and Crystal Structure o f Rare Earth Zinc Borates LnZn(B5O ]0) with Ln = Ce, Nd, Tb  
 Abstract    Single crystals o f the new compounds LnZn(B5O |0) (Ln = (A) C e3+, (B) N d3+, (C) T b '+) were obtained by using a B 20 3 flux technique. X-ray investigations led to space group C2h-P 2,/n (Nr. 14) with lattice parameters: (A) a = 874.5(1), b = 761.4(1), c = 950.0(1), ß = 92.80(1)°, (B) a = 868.6(2), b = 760.9(2), c = 946.0(2), 0 = 92.9 9 (2)°, (C) a = 858.2(2), b = 760.5(2), c = 939.3(2), ß = 93.56(2)°, Z = 4. The structure is isotypic with C oSm (B 5 O |0) and is characte­ rized by two-dimensional infinite 2 (B 5 O 10)5_ ions. Ln is tenfold coordinated by oxygen, and Zn2+ occupies distorted Z n 0 6 polyfiedra. 
  Reference    Z. Naturforsch. 51b, 671—6 (1996); eingegangen am 26. Oktober 1995 
  Published    1996 
  Keywords    Rare Earth, Zinc, Borate, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0671.pdf 
 Identifier    ZNB-1996-51b-0671 
 Volume    51 
114Author    Karsten Bluhm, Andre WieschRequires cookie*
 Title    Synthese und Kristallstruktur von NiHo2(B20 5)2, das erste Nickellanthanoidborat mit einem ^ (B 20 5)4"-Anion Synthesis and Crystal Structure of NiHo2(B20 5)2, the First Nickel Lanthanoid Borates with a (^ (B 20 5)4" A nion  
 Abstract    Single crystals o f N iH o2(B20 5) 2 were prepared by a B20 3 flux-technique in high temperature reactions at 1450 °C and investigated by X-ray diffraction. They crystallize in the space group C 2h-P 2 ,/c (Nr. 14) with a = 451.0(4); b = 724.8(3); c = 938.8(6) pm; ß = 9 1 ,39(1)°; Z = 2. The compound is isotypic to CuTb2(B20 5) 2 as well as to the gadolinite structure (F eY 2 (B e S i0 5)2) and contains a two dimensional infinite anion with the formula 2 (B 2 0 5)4~. The borate layers consist o f four-and eight-membered rings o f edge-sharing B 0 4 tetrahedra. The layers are connected via copper-centered elongated oxygen-octahedra and slightly distorted tetragonal H o 0 8 antiprisms. 
  Reference    Z. Naturforsch. 51b, 677 (1996); eingegangen am 9. November 1995 
  Published    1996 
  Keywords    N ickel, Holmium, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0677.pdf 
 Identifier    ZNB-1996-51b-0677 
 Volume    51 
115Author    Max Herberhold, Guo-Xin Jina, ArnoldL. RheingoldbRequires cookie*
 Title    Sulfur and Selenium Complexes of the Hydrido-tri(3,5-dimethyl-l- pyrazolyl)borate Nitrosylmolybdenum Fragment, [Tp*Mo(NO)]. An X-Ray Crystal Structure Determination of Tp*Mo(NO)(Se5)  
 Abstract    The reactions of hydrido-tri(3,5-dimethyl-l-pyrazolyl)borate nitrosylmolybdenum diiodide, Tp*Mo(NO)L (2), with the oligochalcogenides (N H ^Sio and (NEuteSeö in THF solution lead to mononuclear cvc/o-pentachalcogenido complexes, Tp*Mo(NO)(E5) (E = S (3a), Se (3b)). In the presence of either H2S or H^Se (generated by slow "in situ" hydrolysis of AI2E3 in moist THF solution) 2 is converted into binuclear chalcogenido-bridged products, Tp2Mo2(NO)2(//-E)2 (E = S (4a), Se (4b)) which are more conveniently obtained from 3a,b by dechalcogenation with tri(''butyl)phosphane (1:4,5). The new chalcogen complexes 3a,b and 4a,b were characterized by IR, NMR and mass spectroscopy and compared with the related chalcogen compounds derived from pentamethylcyclopentadienyl nitrosylmolybdenum diiodide, Cp*Mo(NO)l2. The molecular structure of Tp*Mo(NO)(Ses) (3b) has been determined; the complex contains a six-membered MoSe«; metallacycle in the chair conformation and a linearly coordinated nitrosyl ligand (angle M o -N -0 178.9(17)°). 
  Reference    Z. Naturforsch. 51b, 681—685 (1996); received August 28 1995 
  Published    1996 
  Keywords    Molybdenum-chalcogenido Complexes, Nitrosyl Compounds, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0681.pdf 
 Identifier    ZNB-1996-51b-0681 
 Volume    51 
116Author    Manfredo Hörner, Gilberto Antonio, Johannes Pedrosoa, Joachim Beckb, Strähle0Requires cookie*
 Title    Synthese und Struktur von  
 Abstract    A g ^ P h ^ ^ Q H ^ C e n ^ , einem vierkernigen Silber(I)komplex mit l,2-Bis(phenyltriazenido)benzol als Ligand Synthesis and Structure o f A g ^ C P h N ^ C ö R i^ e n h , a Tetranuclear Silver(I) Complex with l,2-Bis(phenyltriazenido)benzene as Ligand Silver(I) Complex, 1,2-Bis(phenyltriazenido)benzene Ligand, Synthesis, Crystal Structure Ag4[(PhN;02C6H4]2(en)2 is obtained by the reaction of [Ag(NHj)2]+ with 1,2-bis-(phenyltriazeno)benzene and ethylenediamine. It crystallizes in the monoclinic space group P2i/c with a = 1064.9(2), b = 2041.8(3), c = 1008.5(3) pm, ß = 101.37(2)°, Z = 2. In the centrosymmetrical tetranuclear complex, the four Ag+ ions form a zigzag chain with Ag-Ag distances of 293.34 and 280.42 pm. Ethylenediamine molecules chelate the two terminal Ag atoms of this chain. Each of the 1,2-bis(phenyltriazeno)benzene ligands in the deprotonated bis(triazenido) form [(PhN^CöPL]2-is bridging three Ag+ ions. The Ag+ ions are coordinated by three N atoms in a trigonal planar arrangement with Ag-N distances between 214.0 and 241.2 pm. 
  Reference    Z. Naturforsch. 51b, 686—690 (1996); eingegangen am 23. Oktober 1995 
  Published    1996 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0686.pdf 
 Identifier    ZNB-1996-51b-0686 
 Volume    51 
117Author    W. Lübbe, W. PreetzRequires cookie*
 Title    undm-[(w-C4H9)4N][B6H5(CH2)2C6H4]  
 Abstract    Preparation, n B, 13C, 'H NM R Spectra and Vibrational Spectra o f 1,2-Xylylene-pentahydro-c/oso-hexaborate, cw-[B6H5(CH2)2C6H4]_ , and the Crystal Structures o f c/s-[P(C6H5)4][B 6H5(CIL,)2C6H4] and c/s-[(n-C4H9)4N ][B 6H5(CH2)2C6H4] 1,2-Xylylene-pentahydro-c/oso-hexaborat(1 -), ' By reaction of [B6H6]2-with u>,u/-dibromo-o-xylene in acetonitrile the 1,2-xylylene-pentahydro-c/oso-hexaborat, ds-[B 6H5(CH2)2C6H4]_ , is formed. The new ansa compound has been separated from excess [B6H6]2-and other reaction products by ion exchange chromatogra­ phy on diethylaminoethyl cellulose. The crystal structures of c/s-[P(C6H5)4][B6H5(CH2)2C6H4] (I) and as-[(n-C4H9)4N][B6H5(CH2)2C6H4] (II) have been determined by single crystal X-ray diffraction analysis: I is monoclinic, space group P 2 \/n with a = 13.715(5), b = 11.118(1) and c = 19.702(2) A, ß = 103.47(2)°; II is orthorhombic with a = 10.204(7), b = 13.352(4) and c = 20.824(8) A. The "B NMR spectrum confirms the structure with a hetero disubstituted octahedral B6 cage with local C2v symmetry. The l3C and 'H NMR spectra have been assigned in term of such a configuration. The IR and Raman spectra exhibit characteristic CH, BH, BC, B6 and arene vibrations. 
  Reference    Z. Naturforsch. 51b, 691—697 (1996); eingegangen am 25. August 1995 
  Published    1996 
  Keywords    H NMR Spectra, Vibrational Spectra, 13C NMR Spectra, 11B NMR Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0691.pdf 
 Identifier    ZNB-1996-51b-0691 
 Volume    51 
118Author    Angeline Stier, Klaus-Jürgen RangeRequires cookie*
 Title    Dicyanometallate, VII [1] Darstellung und Kristallstruktur von Gadolinium-tris-dicyanoaurat (I), Gd[Au(CN)2]3-2,3H20 Dicyano Metallates, VII [1] Preparation and Crystal Structure o f Gadolinium-tris-dicyanoaurate (I), Gd[Au(CN)2]3 -2,3H20  
 Abstract    The title compound has been prepared by adding a stoichiometric amount of gadolinium nitrate hexahydrate to an aqueous solution of potassium dicyanoaurate(I). Single crystals could be obtained by slow evaporation from the saturated solution. The compound crystallizes hexa-gonally, space group P-62m, with a = 6.6319(6), c = 9.108(2) Ä, c/a = 1.3734 and Z = 1. The structure comprises layers of considerably bent dicyanoaurate groups. The gold atoms form a nearly regular 3.6.3.6 -Kagome net with a layer sequence AA.. and an Au -Au distanceoof 3.316(2) A, i. e. remarkably shorter than that found in KAu(CN)2 (Au -Au = 3.652(1) Ä). Above and below the gold layers, the terminal nitrogen atoms of the dicyanoaurate groups build up a two-dimensional net work in the a,b plane, thereby creating trigonal-prismatic holes, which are occupied by the gadolinium ions. Up to three water molecules per unit cell complete the coordination sphere around the gadolinium ion to form a tricapped trigonal prism. The analogous compounds with Ln = Sm, Eu, Tb and Dy are obviously isostructural with the Gd compound, as can be inferred from preliminary X-ray studies. 
  Reference    Z. Naturforsch. 51b, 698—702 (1996); eingegangen am 13. Oktober 1995 
  Published    1996 
  Keywords    Gadolinium-fm-dicyanoaurate(I), Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0698.pdf 
 Identifier    ZNB-1996-51b-0698 
 Volume    51 
119Author    Wolfram Uhlig, HerrnRequires cookie*
 Title    Zur Darstellung neuer Polysiline und vernetzter Polysilane Synthesis of Novel Polysilynes and Branched Polysilanes  
 Abstract    The reductive coupling of halogenated oligosilanes with potassium-graphite leads to novel polysilynes and branched polysilanes. The ratio of quarternary silicon atoms, monoorganosilyl-and diorganosilylgroups in the polymers can be modified by variation in the structure of the starting materials. In this way the properties of the preceramic polymers (molecular weights, solubility, content of carbon, degree of cross-linking) are influenced. The compounds are characterized by 29Si NMR spectroscopy. 
  Reference    Z. Naturforsch. 51b, 703—710 (1996); eingegangen am 18. Dezember 1995 
  Published    1996 
  Keywords    Polysilanes, Polysilynes, Silyltriflates, Potassium-graphite 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0703.pdf 
 Identifier    ZNB-1996-51b-0703 
 Volume    51 
120Author    Na2z, New Sodium, ZincateD. Trinschek, M. JansenRequires cookie*
 Title    Na2Zn02, ein neues Natriumzinkat  
 Abstract    By reacting Na20 , which was produced in situ from NaN3 and NaN02, with reactive ZnO in the solid state, the synthesis of Na2Z n02 has been achieved. Na2Zn02 is metastable up to about 750°C. The novel sodium zincate crystallizes in the spaceogroup P2,/c (No. 14) with the lattice parameters a = 7.7352(2), b = 5.9782(2), c = 5.7248(2)Ä, ß = 94.934(3)°, Z = 4. According to a single crystal structure determination it is an representative of the anti type of the Ln2S20 (Ln = Er, Tm, Yb, Dy) structure. 
  Reference    Z. Naturforsch. 51b, 711—714 (1996); eingegangen am 10. August 1995 
  Published    1996 
  Keywords    Sodium Zincates, Crystal Structure, Metastability 
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 Identifier    ZNB-1996-51b-0711 
 Volume    51 
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