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1996 (295)
41Author    A. Nne, M. Witte, Wolfgang JeitschkoRequires cookie*
 Title    Preparation and Crystal Structure of the Isotypic Carbides Ln3.67TC6 (Ln = rare earth elements; T = Mn, Fe, Ru) and Eu3 ,i6NiC6  
 Abstract    The 14 carbides Ln367MnC6 (Ln = La-Nd) and Ln367TC6 (Ln = La-Nd, Sm; T = Fe, Ru) were prepared from the elem ental components by arc-melting and subsequent annealing. Eu3 16N iC 6 was obtained from a lithium flux. The crystal structures of these nearly isotypic, hexagonal compounds (P63/m, Z = 2) were determined from single-crystal X-ray data; La3 67. FeC6: a = 878.7(2), c = 535.1(1) pm, R = 0.052 for 548 structure factors and 25 variable parameters; Eu316NiC6: a -860.0(1), c = 548.2(2) pm, R = 0.015 for 606 structure factors and 25 variables. The structures differ from the previously reported Gd3Mn2C6 structure by the occupancy of one manganese position by rare earth atoms. Since the lanthanum atoms are larger than the manganese atoms, only two thirds o f these manganese positions can be occupied by the lanthanum atoms in La3 67FeC6. Eu316NiC6 has similar atomic positions. The C-C bond distances in the C2 pairs are 130(2) and 126.5(5) pm in the La and Eu compounds, respectively. Magnetic susceptibility measurements with a SQ U ID m agnetom eter indicate La3 67FeC6 to be Pauli paramagnetic. A test for superconductivity was negative down to 3 K. 
  Reference    Z. Naturforsch. 51b, 249 (1996); received June 12 1995 
  Published    1996 
  Keywords    Lithium Flux, Crystal Structure, Ternary Carbides with C2 Pairs 
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 Identifier    ZNB-1996-51b-0249 
 Volume    51 
42Author    JörgH. Albering, Wolfgang JeitschkoRequires cookie*
 Title    Quaternary Thorium Transition Metal Pnictide Oxides: ThCu^j-PO, ThCuAsO, and Th2Ni3 _xP3 0  
 Abstract    The new compounds T h C u ^ P O and ThCuAsO with ZrCuSiAs-type structure were pre­ pared in well crystallized form by chemical vapor transport reactions. Th2N i3.A :P30 with a new structure type was obtained by reaction o f T h 0 2 with the other elem ental components in an alumina crucible at high temperatures. The crystal structures of the three compounds were determined from single-crystal X-ray data. ThCuj.xPO: P4/nmm, a = 389.43(4), c -828.3(1) pm, R = 0.024 for 13 variable parameters and 338 structure factors; ThCuAsO: P4/ nmm, a = 396.14(5), c = 844.0(1) pm, R = 0.028 (13 variables and 379 F values); Th2Ni3_JP30 : P4/nmm, a = 394.62(4), c = 1723.2(3) pm, R = 0.018 (27 variables and 374 F values). The refinement of the occupancy parameters revealed significant deviations from the ideal values for the transition metal sites for two compounds resulting in the exact compositions ThCu0938(4)PO and Th2N i2 45(nP30 . Magnetic susceptibility measurements indicate Pauli paramagnetism for T hC u^P O . The crystal structures of these compounds are closely related. They belong to a large family o f tetragonal structures of which the ThCr2Si2-and the PbFCl-type structures are well known examples. 
  Reference    Z. Naturforsch. 51b, 257 (1996); received July 6 1995 
  Published    1996 
  Keywords    Crystal Structure, Quaternary Thorium-Transition Metal-Pnictide Oxides, Chemical Vapor Transport 
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 Identifier    ZNB-1996-51b-0257 
 Volume    51 
43Author    PaulK. Baker3, DavidJ M Uldoona, MichaelB. Hursthouseb, SimonJ. Colesb, AidanJ. Laveryc, Andrew ShawcrosscRequires cookie*
 Title    The Crystal Structure and Low Temperature 13C NMR Spectrum of the Seven-Coordinate Complex of Tungsten(II), [WI2(CO)3(NCPh)2]  
 Abstract    The crystal structure of [WI2(C O)3(N C Ph)2] (1) has been determined by X-ray methods. The crystals are orthorhombic, space group Pnam, a = 7.815(3), b = 13.839(5), c = 18.475(3) Ä, Z = 8, R -0.0346 for 1497 observed data. The complex [WI2(C O)3(NCPh)2] has a seven-coordinate geometry, which may be described as a distorted capped octahedron, with the two iodo-ligands mutually trans, while each nitrile is trans to a carbonyl group. The capped octahedral geometry consists of a capping carbonyl (C(10)} on the face defined by 1(1), C(20) and C(20)#. However, the geom etry may also be described as a capped trigonal prism, which has one triangular face occupied by three carbonyl groups and the second triangular face occupied by N (l) , N (l)# and 1(1) atoms, respectively. The iodide 1(2) occupies the capping position on the rectangular face defined by the atoms C(20), C(20)#, N (l), and N (l)# . The low temperature 13C NM R spectrum (203 K, C D 2C12) of 1 shows a single carbonyl resonance at 219.27 ppm which indicates that the com plex is undergoing a rapid fluxional process in solution at 203 K. 
  Reference    Z. Naturforsch. 51b, 263 (1996); received July 7 1995 
  Published    1996 
  Keywords    Crystal Structure, Benzonitrile, Carbonyl, D iiodo, Tungsten(II) 
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 Identifier    ZNB-1996-51b-0263 
 Volume    51 
44Author    G. Jochem, A. Schmidpeter, H. NöthRequires cookie*
 Title    Bis(triphenylphosphoniumyIidyl)phosphane Bis(triphenylphosphoniumylidyl)phosphanes  
 Abstract    Bis(ylidyl)phosphanes can be prepared from ylides and dichlorophosphanes or from bis-(ylidyl)phosphenium chlorides and organolithium compounds. By substituting in bis(ylidyl)-phosphenium chlorides the chloride ion for more basic anions, a large variety o f bis(ylidyl)-phosphanes is accessible. They can be protonated at the ylidic carbon atoms, but alkylated and oxidized at the central phosphorus atom. A s shown by 3IP NM R in solution and by X-ray investigation of the crystal, the lone pair at the tervalent phosphorus is generally oriented synperiplanar to both phosphonio groups. 
  Reference    Z. Naturforsch. 51b, 267—2 (1996); eingegangen am 10. Juli 1995 
  Published    1996 
  Keywords    Ylides, Transylidation, Phosphenium Ions, M ichaelis Arbusov Rearrangement, Diphosphanes 
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 Identifier    ZNB-1996-51b-0267 
 Volume    51 
45Author    Rolf Minkwitz, Ulrike Lohmann, Hans PreutRequires cookie*
 Title    Primäre und sekundäre Ethyl-und /-Propylsulfoniumsalze sowie Kristallstruktur von /-C3H7SH2+SbF6 [1] Prim ary and Secondary Ethyl and /-Propyl Sulfonium Salts and Crystal Structure of /-C3H 7SH2+SbF6-[1]  
 Abstract    The synthesis of salts of the type R"SH3_"+MF6~ (R = C2H 5, i-C3H 7; n = 1, 2; M = As, Sb) by protonation of the corresponding thiols and sulfides in the superacid systems HF/M F5 is reported. The salts have been characterized by vibrational and NM R spectroscopic methods. Isopropylsulfonium hexafluoroantimonate is the first known example of a sulfonium salt, for which a SH bond distance has been determined by a crystal structure analysis, i-C3H 7SH 2+SbF6" crystallizes in the monoclinic space group P2i/m with a = 568.0(4), b = 801.1(6), c = 1019.7(8) pm, ß = 82.63(6) °, with two formula units per unit cell. 
  Reference    Z. Naturforsch. 51b, 277 (1996); eingegangen am 6. Juli 1995 
  Published    1996 
  Keywords    Primary and Secondary Sulfonium Salts, Vibrational Spectra, NM R Spectra, Crystal Structure 
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 Identifier    ZNB-1996-51b-0277 
 Volume    51 
46Author    G. Erhard, Koßmehl* Bettina LabahnRequires cookie*
 Title    Liquid Crystalline Compounds in the Thiophene Series, Part 12+ Synthesis and Characterization of Side Chain Polysiloxanes with Low Transition Temperatures  
 Abstract    Polysiloxanes as side chain polymers containing the 2.2'-bithiophene unit, hexyl and octyl terminal groups and spacer units with 3, 5. 6 and 10 m ethylene groups were prepared and characterized. These polymers have monotropic liquid crystalline phases with transition tem ­ peratures below 0 °C (e. g. for polymer 6p: isotropic — * ■ liquid crystalline transition: -20 °C; liquid crystalline — * ■ solid transition: -43 °C). Polymers with a trimethylene spacer group must contain an octyl terminal group for forming liquid crystalline phase; a hexyl group does not form such a phase. 
  Reference    Z. Naturforsch. 51b, 286—2 (1996); received July 7 1995 
  Published    1996 
  Keywords    Liquid Crystalline Thiophene Compounds, Liquid Crystalline Polysiloxanes, Bithiophene Derivatives, Liquid Crystalline Side Chain Polymers 
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 Identifier    ZNB-1996-51b-0286 
 Volume    51 
47Author    Kuhn3, Thomas Kratz3, G. Erald, H. EnkelbRequires cookie*
 Title    N orbert  
 Abstract    The carbene adduct 5 is formed from the 2-tel-luroimidazoline 4 and iodine. The X-ray structure analysis reveals a dimeric structure in the solid state. 
  Reference    Z. Naturforsch. 51b, 295 (1996); eingegangen am 21. Juli 1995 
  Published    1996 
  Keywords    Tellurium, Carbene, Iodine Reaction, X-Ray 
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 Identifier    ZNB-1996-51b-0295_n 
 Volume    51 
48Author    TabI. Kristalldaten, Frank Weller, Hans-Joachim Mai, Kurt DehnickeRequires cookie*
 Title    D ie Kristallstruktur von [M n(C H 3C N )6][M n I4]  
 Abstract    und Angaben zur Kristallstruktur-bestimmung von [M n(CH3C N)6][MnI4], Crystal Structure of [M n(CH3CN)6][MnI4] M anganese(II) Complex, Crystal Structure, IR Spectra [M n(CH3C N)6][MnI4] crystallizes from aceto-nitrile solutions of M nl2 as yellow single crystals which were characterized by their IR spectrum and by a crystal-structure analysis. Space group P2Jn, Z -4, structure solution with 3742 observed unique reflections with F0 >5cr(F0), R = 0.050. Lattice dim ensions at 20°C: a = 1258.0(5), b = 1244.7(2), c = 1753.3(6) pm, ß = 92.22(3)°. The compound forms octahedral cations [M n(CH3C N)6]2+ with site symmetry Q with average Mn-N bond lengths of 222.3 pm and te­ trahedral anions [M nl4]2' without symmetry with average bond lengths M nl of 271.3 pm. 
  Reference    Z. Naturforsch. 51b, 298 (1996); eingegangen am 13. Juli 1995 
  Published    1996 
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 Volume    51 
49Author    Yoshimitsu Yamazaki, MidoriG. Oto1, ^. Yu-Ichi, Takenori Kageyama, Hiroaki Tomohiro, OkunoRequires cookie*
 Title    Structure of Chloro(cyclopentadienone)- (cyclopentadienyl)ruthenium and its Cytotoxic Activity  
 Abstract    The structure of R u(cpO)(cp)C l com plex (3), which was precipitated from aqueous solutions of R u(cp)2Cl+PF6' (1), was determined by X-ray crystallographic analysis. The Ru-halogen bond distance was shorter and the dihedral angle be­ tween the rings was larger than the values re­ ported for the corresponding Br analogue, R u(cpO)(cp)Br (4). The com plex 3 (IC50 1 09 /iM) was more cytotoxic than 1 (IC50 163 //M) against mouse sarcoma S I80 cells, but less toxic than 4 (IC50 72 ,/M). 
  Reference    Z. Naturforsch. 51b, 301 (1996); received September 21 1995 
  Published    1996 
  Keywords    Ruthenium Complex, Cytotoxicity, X-Ray, Cyclic Voltammetry 
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 Identifier    ZNB-1996-51b-0301_n 
 Volume    51 
50Author    AnneU. Tzolino, K. Arsten BluhmRequires cookie*
 Title    Synthese und röntgenographische Charakterisierung von zwei neuen Verbindungen des Ludwigit-Strukturtyps: Co5Sn(B0 3)2 0 4 und Co5Mn(B0 3 )20 4  
 Abstract    Synthesis and X -R ay C haracterization o f Two New Com pounds with Ludw igite-Structure: C o5S n (B 0 3)20 4 and C o5M n (B 0 3)20 4 The compounds Co5Sn(B 03)20 4 (I) and Co5M n(B03)20 4 (II) were prepared by using a B20 3 flux technique. Single crystals were investigated by X-ray diffraction and showed orthorhombic symmetry, space group D2h-Pbam (No. 55), I a = 944.4; b = 1233.8; c = 310.5 pm; Z = 2 and II a = 925.07; b = 1241.67; c = 305.24 pm; Z = 2. Both compounds are isotypic to the mineral Ludwigite. All metal point positions show an octahedral oxygen coordination. Co2+ and M4+ (M = Sn or Mn) occupy one point position statistically. Both structures contain isolated, trigonal planar B 0 3 units and oxygen atoms that are not coordinated to boron. 
  Reference    Z. Naturforsch. 51b, 305—308 (1996); eingegangen am 28. September 1995 
  Published    1996 
  Keywords    Cobalt, Tin, Manganese, Borate Oxide, Crystal Structure 
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 Identifier    ZNB-1996-51b-0305 
 Volume    51 
51Author    Silke Busche, K. Arsten BluhmRequires cookie*
 Title    Synthese und Kristallstruktur von Dibariumzink-bis(cyclotriborat) Ba2Zn(B30 6)2  
 Abstract    Single crystals of the new compound Ba2Zn(B30 6)2 were obtained by using a B20 3 flux technique. They crystallize in an as yet unknown structure type. X-ray investigations led to space group Cj'-Pl (Nr.2) with lattice parameters a = 715.5(2), b = 720.5(2), c = 1178.9(4), a = 78.96(2)°, /3 = 85.45(2)°, j = 60.12(1)°, Z = 2. The structure is characterized by iso­ lated (B30 6)3_-rings and contains two ninefold coordinated Ba-sites. Zn2+ is tetrahedrally coordinated by oxygen. The relation to the crystal structures of high-temperature BaB20 4 and Ba2Ca(B30 6)2 is discussed. 
  Reference    Z. Naturforsch. 51b, 309—312 (1996); eingegangen am 26. September 1995 
  Published    1996 
  Keywords    Barium, Zinc, Borate, Crystal Structure 
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 Identifier    ZNB-1996-51b-0309 
 Volume    51 
52Author    Park, K. Arsten BluhmRequires cookie*
 Title    Pb6(A s0 4)  
 Abstract    [B (A s04)4] -ein neuartiger Kristallstrukturtyp im System Pb0 /B2 0 3 /As2 0 5 mit einem Beitrag über P b(B A s05) Pb6(A s 0 4)[B (A s 0 4)4] -a New Crystal Structure Type in the System P b 0 /B 20 3/A s20 3 w ith R em arks about P b (B A s0 5) C heong- Single crystals of Pb6(A s04)[B(As04)4] (I) and Pb(BAs05) (II) were obtained by melting B->03, As20 5 and PbO at 800 °C. X-ray investigation led to the space group (I): S4 -P4 (Nr. 81) with a = 715.4(1), c = 976.2(3) pm, Z = 1 and (II): C | -P3, (Nr. 144) with a = 712.2(1), c = 693.5(2) pm, Z = 3. While (II) is isotypic to the Stillwellite structure, Pb^(As04)[B(As04)4] represents a completely novel type of crystal structure. Boron and arsenic are tetrahedrally coordinated by oxygen. These polyhedra form two kinds of isolated anions: A s04'~ and B(A s04)49_. Lead is eightfold coordinated by oxygen. 
  Reference    Z. Naturforsch. 51b, 313—318 (1996); eingegangen am 16. Oktober 1995 
  Published    1996 
  Keywords    Lead, Arsenic, Borate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0313 
 Volume    51 
53Author    Silke Busche, K. Arsten BluhmRequires cookie*
 Title    Ba2KZn3(B306)(B60 13)  
 Abstract    Single crystals of the new compound Ba2KZn3(B30 6)(B60 | 3) were obtained by using a B20 3 flux technique; they crystallize in an as yet unknown structure type. X-ray investigations led to the space group C '-P l (Nr.2) with lattice parameters a = 705.2(2), b = 712.5(2), c = 1880.3(6), a = 93.43(3)°, ß = 90.72(2)°, 7 = 119.57(2)°, Z = 2. The structure contains (B30 6)3~-rings and a new discrete (B60 13)8~ anion, which is composed of two B 0 4 and two B20 5 units. Zn-+ is tetrahedrally coordinated by oxygen and two out of three tenfold coordinated Ba-sites are statistically occupied by Ba2+ and K+. 
  Reference    Z. Naturforsch. 51b, 319—324 (1996); eingegangen am 26. September 1995 
  Published    1996 
  Keywords    Barium, Potassium, Zinc, Borate, Crystal Structure 
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 Identifier    ZNB-1996-51b-0319 
 Volume    51 
54Author    H. Einer, HomborgRequires cookie*
 Title    Inin -Phthalocyanine: Darstellung, Eigenschaften und Kristallstruktur von £-Bis(triphenylphosphin)iminium-as-di(cyanato(N))phthalocyaninato- (2-)indat(III)  
 Abstract    In111 Phthalocyanines: Synthesis, Properties and Crystal Structure of Z?-Bis(triphenylphosphine)iminium c/5-D i(cyanato(N))phthalocyaninato(2-)indate(III) B arbara Aßm ann, A ndreas Franken, [In(Cl)Pc2~] reacts with bis(triphenylphosphine)iminium cyanate ((PNP)OCN) in dichlo-romethane to yield green-blue *(PNP) [In(NCO)2Pc2_] • CH2C12, which crystallizes in the triclinic space group Pi (No. 2) with Z = 2. The two cyanato(N) ligands are in a mutually cis coordination (Z (NNCO-In -N NCO) = 84.2(3)°). The In atom is displaced out of the plane of the four N,.vo atoms towards the two cyanato(N) ligands (d(In-Ct(N,JO)4) = 0.988 A). The average In-N NC0 and In-N,.so bond distances are 2.16(1) and 2.216(8) A, respectively. The NNco-In -NNCO moiety deviates by ~ 4° from the staggered conformation relative to the In-(N,,")4 sceleton. Though the cyanato(N) ligands are essentially linear, there are different In-N -C angles (164.4(9) and 147.1(8)°) probably due to crystal packing effects. The Pc2~ ligand is distorted in an asymmetrically convex manner. The PNP cation adopts the bent conformation (Z(P-N(K)-P) = 143.5(6)°). The cyclic voltammogram shows three electrode processes, which are assigned to the redox pairs: Pc ~/Pc2~ (-0.87 V) < In'/In111 (-0.63 V) < Pc~_ /Pc~ (0.69 V). The UV-VIS-NIR spectra and the vibrational spectra are discussed. 
  Reference    Z. Naturforsch. 51b, 325—332 (1996); eingegangen am 21. August 1995 
  Published    1996 
  Keywords    Indium(III) Phthalocyanines, Cyanato(N) Complex, Cyclic Voltammetry, Crystal Structure, Optical and Vibrational Spectra 
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 Identifier    ZNB-1996-51b-0325 
 Volume    51 
55Author    D. Frerichs, C. H. Park, HkM. Üller-B, UschbaumRequires cookie*
 Title    Zur Kenntnis zweier Formen des Zinkorthoarsenates: a-Z n 3(A s04)2 und /3-Zn3(A s0 4)2 On Two Forms o f Zinc O rthoarsenate: a -Z n 3(A s 0 4)2 and /3-Zn3(A s 0 4)2  
 Abstract    Single crystals of two forms of zinc orthoarsenate (a-Z n3(A s04)2 (I) and /3-Zn3(A s04)2 (II)) have been prepared by flux techniques. Both compounds crystallize monoclinically, space groups (I): Cih-P2l/c, (II): Cih-P21/n, with the lattice parameters (I): a = 6.306(2), b = 8.652(2), c = 'ol 1.321(4) A, ß = 92.25(5) °, Z = 4 and (II): a = 5.281(1), b = 8.494(2), c = 7.726(3) A, ß = 96.39(3)°, Z = 2. ct-Zn3(A s04)2 is isotypic to I-Cu3(A s04)2 and ß-Zn3(A s04)2 to 7-Zn3(P 0 4)2. Similarities and differences of the crystal structures are discussed. 
  Reference    Z. Naturforsch. 51b, 333—337 (1996); eingegangen am 31. August 1995 
  Published    1996 
  Keywords    Zinc, Arsenic, Oxide, Crystal Structure 
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 Identifier    ZNB-1996-51b-0333 
 Volume    51 
56Author    O. Sfreddo, Ch Rabbow, HkM. Üller-B, UschbaumRequires cookie*
 Title    Eine neue Verbindung im System Ba/Ln/Zn/Pt/O: Bs^Sn^Zi^PtOis On a New Com pound in the System B a/Ln/Zn/Pt/O : Ba4Sm 4Z n3P tO |5  
 Abstract    Reactions of mixtures of B aC 03, ZnO, Sm20 3 (3:5: 1) heated in platinum crucibles up to 1250 °C led to big black single crystals of Ba4Sm4Zn3P t0 15. The new compound crystallizes with hexagonal symmetry, space group C^-Pö^mc, a = 1 L657, c = 6,789 A , Z = 2. It is isotypic with Ba6Nd2Al4O l5 but shows an ordered Pt4+ and Zn2+ distribution over the aluminium positions. The octahedrally coordinated barium sites of the Ba6Nd2Al40 15 type are occupied by Sm3+. In comparison to compounds of the composition Ba6Ln2M40 15 (M = Al, Fe, Co), Ba4Sm4Zn3PtOi5 is the first example containing different oxidation states at the M '+ positions. 
  Reference    Z. Naturforsch. 51b, 338—342 (1996); eingegangen am 22. August 1995 
  Published    1996 
  Keywords    Barium Rare Earth, Zinc, Platinum, Oxide, Crystal Structure 
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 Identifier    ZNB-1996-51b-0338 
 Volume    51 
57Author    Ch Rabbow, HkM. Üller-B, UschbaumRequires cookie*
 Title    Zur Kenntnis eines Barium-Lanthanoid-Aluminat-Zinkats: BaLuAlZn30 7 mit einem Anhang zu Ba2Er2Zn80 13  
 Abstract    Reactions of B aC 03, ZnO, Lu20 3 and A120 3 mixtures at temperatures up to 1500 °C led to small and colourless rods of BaLuAlZn30 7. The new compound crystallizes with hexagonal symmetry, space group CöV -P63mc, a = 6.273, c =10.161 A, Z = 2. In spite of small differences in the oxygen content BaLuAlZn30 7 is isotypic to Ba2Ln2Zn80 13. The crystal structure shows Zn2+ with tetrahedral, Lu '+ with octahedral and Ba:+ with anticuboctahedral coordination by 0 2~. It has been shown that parts of the [Zn3A107]5_ network are fragments of the ZnO structure. In consequence one oxygen atom is fourfold coordinated by zinc/aluminium. The space group of Ba2Ln2ZnxO i3 must be corrected to C6V -P63mc. 
  Reference    Z. Naturforsch. 51b, 343—347 (1996); eingegangen am 27. Juli 1995 
  Published    1996 
  Keywords    Barium, Rare Earth, Zinc, Aluminium, Crystal Structure 
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 Identifier    ZNB-1996-51b-0343 
 Volume    51 
58Author    Jörg Laue, G. Unther Seitz, H. Ans, W. AßmuthRequires cookie*
 Title    Synthese und [4+2  
 Abstract    ]-Cycloadditionen von 4a, 8a-Methanophthalazin, das erste Propellan mit einem elektronenreichen und einem elektronenarmen 47r-Diensystem Synthesis and [4+2] C ycloaddition Reactions o f 4a, 8a-M ethanophthalazine, the First Propellane w ith an E lectronrich and an Electrondeficient 47r-Diene System Cyclopropabenzene 3 reacts with 3,6-bis(trifluoro)-l,2,4,5-tetrazine 4 to afford in high yield the 4a,8a-methanophthalazine 6, the first propellane, containing an electron rich cyclohexadiene system on the one hand and an electron deficient diazadiene system on the other hand. According to the principle of Diels-Alder reactions with inverse electron demand, electron rich dienophiles like ketene acetals, enamines or dimethyl hydrazones react predominantly with the diazadiene system to yield the azo-bridged cycoadducts of type 19 and/or the tricyclic tetrahydropyridazines like 20. In the same fashion several more or less angle strained cycloalkenes cycloadd to the diazadiene of the propellane 6 to give the novel polycyclic azo compounds 34, 36, 38,40, 42 and 44 with exo-configuration of the annulated cycloalkanes. Attack apparently occurs from less hindered face anti to the methano bridge of 6 with high stereo-and site-selectivity. As anticipated the electron deficient dienophiles 1,2,4-triazoline-3,5-dione 45 and the benzoquinone 46 add with different site selectiviy to 6 furnishing the polycyclic pyridazines 47 and 48 resp. again by exclusive anti attack. Treatment of 6 with both an electron rich and an electron deficient dienophile like 49 and 45 resp. affords the heptacyclic anti-anti-bis adduct 51 with analogously high site-and stereoselectivity. 
  Reference    Z. Naturforsch. 51b, 348—358 (1996); eingegangen am 31. August 1995 
  Published    1996 
  Keywords    Diels-Alder Reactions, Valence Tautomerism, Propellane, Bivalent, 7r-Facial Selectivity, Site Selectivity 
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 Identifier    ZNB-1996-51b-0348 
 Volume    51 
59Author    W. Lübbe, W. PreetzRequires cookie*
 Title    Darstellung, n B-, 13C-, ^ -N M R -und Schwingungsspektren von ji-Pentamethylen-bis  
 Abstract    hexahydro-c/oso-hexaborat, [B6H6(CH2)5B6H6]2', und ji-Hexamethylen-bis-hexahydro-c/oso-hexaborat, [B6H6(CH2)6B6H6]2 Preparation, n B, l3C, 'H NMR and Vibrational Spectra of /x-Pentamethylene-bis-hexahydro-c/oso-hexaborate, [B6H6(CH2)5B6H6]2_, and /i-Hexamethylene-bis-hexahydro-c/<m>-hexaborate, [BftH ötC^^BftH ö]2- /i-Pentamethylene-bis-hexahydro-c/o5<7-hexaborate(2-), /u-Hexamethylene-bis-hexahydro-c/cw-hexaborate(2-), ' 
  Reference    Z. Naturforsch. 51b, 359—362 (1996); eingegangen am 7. September 1995 
  Published    1996 
  Keywords    H NMR Spectra, l3C NMR Spectra, "B NMR Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0359.pdf 
 Identifier    ZNB-1996-51b-0359 
 Volume    51 
60Author    W. Lübbe, W. PreetzRequires cookie*
 Title    Darstellung, n B -,13C -,1 H-NMR-und Schwingungsspektren von ja-Dimethylen-bis  
 Abstract    hexahydro-c/oso-hexaborat, [B6H6(CH2)2B6H6]2', sowie Kristallstrukturen von [As(C6H5)4]2[B6H6(CH2)2B6H6] [(CH3)2CO] und [P(C6H5)4]2[B6H6(CH2)2B6H6][C 2H5OH] Preparation, " B , 13C, 'H NM R and Vibrational Spectra of /i-Dimethylene-bis-hexahydro-c/oso-hexaborate, [BeHöCCI^hBöHö]2" , and the Crystal Structures o f [As(C6H5)4]t[B 6H6(CH2)2B 6H6] [(CH3)?CO] and [P(C6H5)4]2 [B6H6(CH2)2B6H6] • [C2H5OH] ^-Dimethylene-bis-hexahydro-c/as'o-hexaborate(2- By reaction of [B6H6]2~ with dibromoethane in acetonitrile /j-dimethylene-bis-hexa-hydro-c/oso-hexaborate(2-), JBfiHötCfLbBfcHö]2 -, is formed. The compound was sepa­ rated from excess [B6H6]'_ by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structures of [AstCfiH.^MBöHötCHbhBöHftl-IXCI-L^CO] (I) and [P(Cf,H5)4]2[BftH^CHT^BftHf,]■ [C2H5OH] (II) have been determined by single crystal X-ray ana­ lysis: I is triclinic, space group PI with a = 10.264(2), b = 13.804(2) and c = 20.242(2) A, a = 97.857(10)°, ß = 92.734(11)° and 7 = 103.024(13)°; II is monoclinic, space group P2iIn with a = 12.742(2), b = 7.532(2) and c = 26.887(3) Ä, ß = 95.765(10)°. The 11B NMR spectrum of this compound reveals the feature of monosubstituted octahedral B6 cages. The l3C NMR spectrum exhibits a triplet at 16.20 ppm with '7(C,H) = 120.4 Hz. In the 'H NMR spectrum a singulet at 0.72 ppm of the CH2-groups and two singulets at 1.72 and -4.95 ppm of the BH fragments are observed. The IR and Raman spectra exhibit strong CH stretching bands between 2908 and 2789 cm-1, BH stretching bands between 2463 and 2396 cm-1, and the BC stretching vibration at 1144 in the IR and at 1150 cm" 1 in the Raman spectrum. 
  Reference    Z. Naturforsch. 51b, 363—369 (1996); eingegangen am 3. August 1995 
  Published    1996 
  Keywords    ), Crystal Structure, 'H NMR Spectra, Vibrational Spectra, l3C NMR Spectra, "B NMR Spectra 
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 Identifier    ZNB-1996-51b-0363 
 Volume    51 
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