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1995[X]
41Author    R. Oland Eger, R. Einhard, K. K. Rem Er, A. Rn, T. SimonRequires cookie*
 Title    Y7 I1 2 C2 N: Eine Verbindung aus Einheiten zweier Y6 (C2)-Oktaeder und eines Y6 N 2-Tetraederdoppels  
 Abstract    Y 7 Ii2C2N: A C om pound with U nits of Two Y 6(C 2) O ctahedra and a Y 6N 2 D ouble T etrahedron H ansjürgen M attausch, H orst B o rrm an n , The new compounds Y7I12C2N and H o7I 12C2N have been prepared by reaction of stoi­ chiometric amounts of the metals (R E), R E I3, REN and C in closed Ta capsules at 1150 and 1120K, respectively. Pure samples of the compounds were obtained after 5 days annealing time. The crystals with xenomorphic shape are olive-green (Y7I12C2N) or red-brown (H o7I I2C2N) in colour and sensitive to air and moisture. Y7I 12C2N crystallizes in the space group P I (No. 2) with lattice constants a = 971.24(7), b = 1030.38(7), c = 1673.58(11) pm and a = 101.366(5), ß = 92.758(5), y = 112.799(5)°. According to Guinier photographs H o7I12C2N is isotypic with the lattice consiants u -968.8(3), b = 1028.7(3), r. = 1667.8(5) pm and a = 101.31(2), ß = 92.78(2), y = 112.80(1)°. In the structure the C atoms are present as C2 units with a C -C distance of 144 pm. These C2 units are octahedrally coordinated by Y atoms (o x). The N atoms are in the center of Y4 tetrahedra, which are linked via a com mon edge to form double tetrahedra (t2). By condensa­ tion of N-centered double tetrahedra (t2) with a C2-centered Y octahedron (01) the character­ istic units Ojt2Oi are formed. The I atom s coordinate all free edges and corners of these units and connect them via I '-I ° contacts parallel [100] and [001]. The compounds are semiconducting. H o7I12C2N exhibits Curie-Weiss behaviour with 6 = 15(1) K and ue({ = 10.5(1) f.iB. 
  Reference    Z. Naturforsch. 50b, 931—936 (1995) 
  Published    1995 
  Keywords    Yttrium Iodide Carbide Nitride, Holmium Iodide Carbide Nitride, Crystal Structure 
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 Identifier    ZNB-1995-50b-0931 
 Volume    50 
42Author    R. Ainer PöttgenRequires cookie*
 Title    EuPdGe -a New Germanide with EuNiGe Type Structure  
 Abstract    The title compound was prepared from the elem ental com ponents in a tantalum tube at 1070 K and investigated by X-ray diffraction of both powder as well as single crystals. The crystal structure was refined from four-circle diffractometer data: P 2 xln, a = 618.1(1), b = 613.6(1), c = 743.9(1) pm, ß = 109.40(1)°, V = 0.2661(1) nm3, Z = 4 ,w R 2 = 0.0536 for 1564 F2 values and 29 variables. EuPdGe crystallizes with the E uN iG e type structure. Both Pd and G e atom s in EuPdGe have three germanium or palladium neighbors, respectively. They form two-dim ensionally infinite [PdGe] polyanions which consist o f corrugated 4.82 nets. These polyanions are separated by the europium atoms. 
  Reference    Z. Naturforsch. 50b, 1181—1184 (1995); received March 1 1995 
  Published    1995 
  Keywords    Germanide, Crystal Structure, X-Ray, Europium 
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 Identifier    ZNB-1995-50b-1181 
 Volume    50 
43Author    KatrinA. Köhler, H. Lexander Steiner, W. Erbert, RoeskyRequires cookie*
 Title    Die Kristallstrukturen von (j75-C5Me5)MoMe4 und (j75-C5Me5)WMe4 The Crystal Structures of (?75-C5Me5)M oMe4 and (^5-C5Me5)W M e4  
 Abstract    The crystal structures of (/75-C5Me5)MoMe4 1 and (j/5-C5Me5)WMe4 2 are reported. 1 and 2 crystallize in the orthorhom bic space group Pbcm with the lattice param eters a = 681.4(2) pm, b = 1538.6(6) pm, c = 1402.4(6) pm with 4 units per cell (1), and a = 684.99(6) pm, b = 1547.3(2) pm, c = 1405.5(2) pm with 4 units per cell (2). Both compounds are monomeric and have a square-pyramidal geometry. 
  Reference    Z. Naturforsch. 50b, 1207—1209 (1995); eingegangen am 20. Januar 1995 
  Published    1995 
  Keywords    Molybdenum, Tungsten, Alkyl Complexes, Crystal Structures 
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 Identifier    ZNB-1995-50b-1207 
 Volume    50 
44Author    Z. NaturforschRequires cookie*
 Title    Hexacarbonyldieisen-stabilisierte Sulfimid-Derivate, Fe2(CO)6(w-SNR)  
 Abstract    Hexacarbonyl diiron com plexes of N-substituted sulfimides (SN R) have been obtained from the parent tetrahedrane, Fe2(C O)6(//-SN H) (1), by deprotonation to give the anion Fe2(C O)6(/i-SN _) (2) and subsequent reaction with either trialkyloxonium or carbenium tetrafluoroborates. The new aza-diferra-thia-tetrahedranes, Fe2(C O)6(w-SNR) (R = CH3 (3a), C2H5 (3b), CPh3 (3c), cyc/o-C^Ph^ (3d), cyclo-C 7H 7 (3e), and cyc/o-(C7H 7)M (CO)3 with M = Cr (3f), Mo (3g), W (3h)) were characterized by their 'H and 13C NM R as well as their IR and MS spectra. The molecular structure of Fe2(C O)6[S N -cy c/o -C 7H 7M o(C O)3] (3g) has been determined by X-ray diffraction. 
  Reference    Z. Naturforsch. 50b, 1252—1556 (1995); eingegangen am 29. Dezem ber 1994 
  Published    1995 
  Keywords    Sulfimide Complexes, Hexacarbonyl Diiron Complexes, Crystal Structure 
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 Identifier    ZNB-1995-50b-1252 
 Volume    50 
45Author    M. Arietta, S. Schriewer-Pöttgen, Wolfgang JeitschkoRequires cookie*
 Title    Two Modifications of Hg5Re2O 10  
 Abstract    The previously reported mercury perrhenate Hg5 Re2O 10, prepared hydrothermally, has now been obtained by reaction of HgO with the mercury(II) metaperrhenate H g (R e 0 4)2 in sealed silica tubes. A second modification o f this compound can be obtained by reaction of elem ental mercury with H g (R e 0 4)2 also in sealed silica tubes. Its crystal structure has been determined from single-crystal X-ray data: P 2 x/c, a -861.5(1), b = 1200.9(2), c = 1203.9(2) pm, ß = 97.15(1)°, Z = 4, R = 0.024 for 1733 structure factors and 105 variables. Both modifi­ cations may be represented by the formula H g2+-2H g20 -2 R e 0 4_, indicating that mercury occurs in oxidation states I and II. In both modifications the mercury and some oxygen atoms form two-dimensionally infinte, puckered, cationic nets of the composition (H g2+-2H g20)" , which are separated by the R e 0 4~ tetrahedra. In the modification reported earlier the mer­ cury oxygen nets consist of condensed 16-membered rings, while the nets of the present modification contain 10-and 22-membered rings. 
  Reference    Z. Naturforsch. 50b, 1335—1339 (1995); received February 27 1995 
  Published    1995 
  Keywords    Crystal Structure, Mercury Perrhenates, Phase Transitions 
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 Identifier    ZNB-1995-50b-1335 
 Volume    50 
46Author    R. Upert Marx3, HansMichael MayerbRequires cookie*
 Title    Reindarstellung und Kristallstruktur von Lithiumnitriddibromid, Li5NBr2 Preparation and Crystal Structure of Lithium Nitride Dibromide, Li5N B r2  
 Abstract    Single phase Li5NBr2 was prepared by the reaction of Li3N and dry, O H -free LiBr under inert gas at 430 °C. In the quasi-binary system Li3_2*Ni_ vB rir, Li5NBr2 is the second most nitride rich compound after Li10N 3Br. Following unit cell indexing using laboratory X-ray powder data the previously unknown structure o f Li5NBr2 was solved from neutron powder diffraction data recorded at the flat-cone and powder diffractometer E 2 at the rebuilt reactor BER II in Berlin. The title compound crystallizes in the orthorhombic space group Immm (No. 71), a = 603.79(4), b -1181.3(1), c = 390.14(3) pm with two formula units per unit cell. The L i-N -sublattice comprises linear chains of vertex sharing Li6N-octahedra which are aligned along the short c-axis and are separated by chains o f bromine atoms. The N -B r arrangement may be regarded as an ordered A X 2 variant o f a cubic close packing involving two kinds of atoms. Lithium atoms occupy the tetrahedral holes formed by one nitrogen and three bromine atoms, as well as the N -N edges of the N 2Br2 tetrahedra. 
  Reference    Z. Naturforsch. 50b, 1353—1358 (1995); eingegangen am 16. Februar 1995 
  Published    1995 
  Keywords    Lithium Nitride Dibromide, Preparation, Crystal Structure 
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 Identifier    ZNB-1995-50b-1353 
 Volume    50 
47Author    Z. NaturforschRequires cookie*
 Title    Aminolyse von Cp2ZrCl{P(SiMe3)2} -Synthese und Molekülstruktur von Cp2ZrCl(NHPh)  
 Abstract    The reaction of Cp2ZrCl{P(SiM e3)2} with aniline yields the terminal zirconocene phenyl­ amido com plex Cp2Z rCl(N H Ph) (1) and H P(SiM e3)2. 1 was characterized spectroscopically (n.m.r., i.r.) and by X-ray structure determination (monoclinic space group P 2 {ln, a -6.589(2), b = 19.978(3), c = 13.512(2) Ä , ß = 101.09(2)° (at 200 K)). The NHPh group is planar with Z r -N 2.116(10) A. 
  Reference    Z. Naturforsch. 50b, 1359—1361 (1995); eingegangen am 24. Februar 1995 
  Published    1995 
  Keywords    Aminolysis, Zirconocene Phosphido Complex Zirconocene Phenylamido Complex, Crystal Structure 
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 Identifier    ZNB-1995-50b-1359 
 Volume    50 
48Author    CsO. Rb, H.-Jürgen Laf Reckeweg, MeyerRequires cookie*
 Title    A4[Nb6Cl12(N3)6](H20 ) 2 mit A = Rb, Cs Synthesis and Structure of the Cluster Azides: A ^N böCl^N O öK IH bO ^ with A =  
 Abstract    The new compounds A4[Nb6Cli2(N3)6](H:0)2 (A = Rb, Cs) were synthesized from In4[Nb6Cli2Cl6] by substituting six terminal Cl ligands and the In+ ions in methano-lic solution. An X-ray structure refinement was performed on single-crystal data of Rb4[Nb6Cli2(N3)6](H?0)2 (1) (space group Pi, Z = 1, a = 912.5(1) pm, b = 937.2(1) pm, c = 1062.0(1) pm, a = 96.88(2)°, ß = 101.89(1)°, 7 = 101.44(2)°) and Cs4[Nb6Cli2(N3)6](H20)2 (2) (space group PI, Z = 1, a = 920.9(5) pm, b = 947.9(7) pm, c = 1091.8(7) pm, a = 96.89(6)°,/?= 103.35(5)°, 7 = 101.60(5)°. Each of the centrosymmetric [Nb6Cli2(N3)6]4~ ions of the isotypic compounds contains six terminal azide groups at the corners of the octahedral niobium cluster (dfvj^N = 226(1) pm (1), 225(1) pm (2), bond angles Nb-N-N 120-127°). The [Nb6Cli2(N3)6]4_ ions are linked via Rb-N and Rb-Cl interactions of the Rb+ ions to form a three-dimensional structure. Crystals of the compounds react explosively on heating or mechanical pressure. Die Synthese und Struktur von Clusteraziden: 
  Reference    Z. Naturforsch. 50b, 1377—1381 (1995); eingegangen am 16. Januar 1995 
  Published    1995 
  Keywords    Niobium Cluster Azides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1995-50b-1377 
 Volume    50 
49Author    Karl-Friedrich Tebbe3, MervatEl Essawib, Sawsan Abd, El KhalikbRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XIX [1]  
 Abstract    Bis(methyltriphenylphosphonium)oktaiodid (M ePh3P)2I8, Cäsium(18-Krone-6)triiodid [Cs(C12H 24 0 6)]I3, Iodoblei(18-Krone-6)triiodid [Pb(C12H2406I]I3 und Diiodothallium(18-Krone-6)tetraiodothallat [T1(C12H240 6)I2](T1I4) Studies of Polyhalides, XIX [1] Bis(methyltriphenylphosphonium) Octaiodide (M ePh3P)2I8, Cesium(18-crown-6) Triiodide [Cs(C12H 240 6)]I3, Iodolead(18-crown-6) Triiodide [Pb(C 12H 240 6)I]I3 and Diiodothallium(18-crown-6) Tetraiodothallate [T1(C12H 240 6)I2](T1I4) (M ePh3P)2l 8 has been prepared by the reaction of methyltriphenylphosphonium iodide with iodine in ethanol. It crystallizes in the m onoclinic space group P 2 xln with a = 985.2(2), b = 1260.0(1), c -1872.6(4) pm, ß = 91.50(2)° and Z = 4. The crystal structure has been refined to R = 0.030 for 2882 reflections. It may be described as a layerlike packing of cations and anions. The anion with point symmetry 1 consists o f two triiodide groups and a bridging iodine molecule forming a rather comm on nearly planar Z-shaped octaiodide ion I82". [Cs(18-crown-6)]I3 has been prepared by the reaction of cesium_iodide and 18-crown-6 with iodine in ethanol. It crystallizes in the triclinic space group PI with a = 921.4(1), b = 1175.4(7), c = 1178.0(4) pm, a = 112.82(4), ß = 94.24(7), y = 98.60(3)° and Z = 2. The crystal structure has been refined to R = 0.038 for 3302 reflections. The geom etry of the cation [Cs(18-crown-6)]+ and of the anion I3~ is quite normal. [Pb(18-crown-6)I]I3 has been prepared by the reaction of lead iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the m onoclinic space group P 2 j/a7 with a = 833.6(3), b = 1721.0(6), c = 1730.6(6) pm, ß = 99.61(3)° and Z = 4. The crystal structure has been refined to R = 0.047 for 2772 reflections. It consists o f com plex cations [Pb(18-crown-6)I]+ and triiodide anions I3_ forming weakly bonded ion pairs. [Tl(18-crown-6)I2](TlI4) has been prepared by the reaction of thallium (I)iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the m onoclinic space group P 2 xln with a = 1236.8(3), b = 1382.6(3), c = 1710.2(2) pm, ß = 90.76(1)° and Z = 4. The crystal structure has been refined to R = 0.044 for 2916 reflections. It is com posed o f com plex cations [Tl(18-crown-6)I2] + nd complex anions TII4_ with their usual and expected geometry. 
  Reference    Z. Naturforsch. 50b, 1429—1439 (1995); eingegangen am 4. Oktober 1994 
  Published    1995 
  Keywords    Triiodides, Octaiodide, Tetraiodothallate, Crown Ether Complexes, Crystal Structures 
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 Identifier    ZNB-1995-50b-1429 
 Volume    50 
50Author    Karl-Friedrich Tebbe, Taraneh FaridaRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XX [1]  
 Abstract    Darstellung und Kristallstruktur von Tetra(m ethyltriphenylphosphonium)docosaiodid (M ePh3P)4I22 Studies of Polyhalides, XX [1] Preparation and Crystal Structure of Tetra(methyltriphenylphosphonium)docosaiodide (M ePh3P)4I22 The new compound (M ePh3P)4I22 has been prepared by the reaction of Ph3MePI with iodine in a mixture of methanol and dichloromethane. It crystallizes in the triclinic space group P i with a = 1018.4(3), b = 1333.0(4), c = 2042.9(6) pm, a = 88.56(2), ß = 78.05(2), y = 76.03(2)° and Z = 1. The crystal structure has been refined to RF = 0.0487 for 5525 reflections. It may be described as a layer-like packing of cations [CH3(C6H3)3P]+ and anions I224-di­ vided in one I)22-and two I5_ groups. The central Ii22-anion with point symmetry Q consist­ ing of two L-shaped pentaiodide groups and a bridging iodine molecule is completed by two further end-on bonded pentaiodide ions with a rather short distance o f 366.7(2) pm to the weakly bonded and nearly isolated docosaiodide ion. 
  Reference    Z. Naturforsch. 50b, 1440—1444 (1995); eingegangen am 6. März 1995 
  Published    1995 
  Keywords    Methyltriphenylphosphonium Ion Polyiodide, D odecaiodide D ocosaiodide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1440 
 Volume    50 
51Author    N., Silke Busche, Karsten BluhmRequires cookie*
 Title    Synthese und Kristallstruktur der ersten zinkhaltigen Pyroborate  
 Abstract    ii,5Z n 0,5(6 2 0 5) UI,d C o ^ Z n o ^ I ^ O s) Synthesis and Crystal Structure of the First Zinc Containing Pyroborates Nii.5Z n0.5(B2O 5) and Coj 5Z n0.5(B2O 5) The first zinc containing pyroborates Ni! sZ n ^ B ^ O s) (A) and 5Zn0 5(B 2O 5) (B) were prepared by using a B20 3 flux technique. Single crystals were investigated by X-ray diffrac­ tion and showed triclinic symmetry, space group C j-P l. The structures are isotypic to C o9(B 20 5) with the lattice parameters (A) « = 331.28(6), 6 = 613.87(11), c = 922.2(2), a = 104.067(11) °, ß = 90.672(13) °, y = 92.413(12) 0 and (B) 0 = 315.89(2), 6 = 612.84(6), c = 927.72(6), a = 104.103(7) °, ß = 91.020(6) °, y = 92.540(7) °, Z = 2. All metal point positions show an octahedral oxygen coordination and a partly statistical distribution o f Zn2+ and N i2+ or C o2+, respectively. Isolated nearly planar B20 5 units connect ribbons consisting o f edge sharing metal octahedra. 
  Reference    Z. Naturforsch. 50b, 1445—1449 (1995); eingegangen am 25. April 1995 
  Published    1995 
  Keywords    Zinc, Nickel, Cobalt, Pyroborate, Crystal Structure 
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 Identifier    ZNB-1995-50b-1445 
 Volume    50 
52Author    Silke Busche, Karsten BluhmRequires cookie*
 Title    Zur Synthese und Kristallstruktur von Zinkboratoxiden mit isolierten, trigonal planaren B 0 3-Baugruppen: Zn5M n(B03)20 4 und Z nF e(B 03) 0 Synthesis and Crystal Structure of Zinc Borate Oxides Containing Isolated Trigonal Planar B 0 3 Units: Z n5M n (B 0 3)20 4 and Z n F e(B 0 3) 0  
 Abstract    Single crystals of the new compounds Zn5M n (B 0 3)20 4 (A) and Z n F e (B 0 3) 0 (B) were prepared by using a B20 3 flux technique. Zn5M n (B 0 3)20 4 is isostructural with Ni5T i(B 0 3)20 4 and Z n F e (B 0 3) 0 is isotypic with the mineral warwickite. X-ray investiga­ tions on single crystals led to (A) space group D ^ -P b a m , a = 926.41(10), b = 1236.67(8), c = 304.55(3) pm, Z = 2, and (B) space group D i^ -P n m a, a = 924.62(4), b = 314.1(10), c = 935.3(2) pm, Z = 4. The structure o f Zn5M n (B 0 3)20 4 (A) contains four octahedrally coordi­ nated metal sites, one of these statistically occupied by Zn2+ and Mn4+. In the structure o f Z n F e (B 0 3) 0 the ions Zn2+ and Fe3+ occupy statistically both distorted octahedral sites. Both structures contain isolated B 0 3 units and oxygen that is not coordinated to boron. 
  Reference    Z. Naturforsch. 50b, 1450—1454 (1995); eingegangen am 25. April 1995 
  Published    1995 
  Keywords    Zinc, Manganese, Iron Borate Oxide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1450 
 Volume    50 
53Author    A.Rnd Müller, Gerald Henkel, ThiolatoRequires cookie*
 Title    [Ni2(SC4H9)6]2-> ein neuartiger zweikerniger Nickel-Thiolato-Komplex mit kantenverknüpften NiS4-Tetraedern und [Ni(SC6H4SiMe3)4]2-, ein strukturchemisch verwandtes einkerniges Komplexion [Ni2(SC4H 9)6]2~, a Novel Binuclear Nickel-Thiolat Complex with NiS4 Tetrahedra Sharing Edges and [Ni(SC6H4SiMe3)4]2_, a Structurally Related M ononuclear Complex Ion  
 Abstract    Reaction of nickel(II) chloride with sodium or potassium tert-butane thiolate in acetonitrile affords the isotypical compounds [Nb(SrC4H9)6]Na2 • 4 MeCN (1) and [Ni7(SfC4H9)6]KT • 4 MeCN (2), respectively. Crystal data: 1: a = 9.859(3), b = 11.877(3), c = 19.675(5) Ä , ß = 96.11(2)°, space group P 2x/n, Z = 2:2: a = 9.854(2), b = 11.915(3), c = 20.558(5) Ä , ß = 99.62(2)°, space group P 2xln, Z = 2. The structures were refined to R = 0.0599 (1) and 0.0562 (2), respectively. Both compounds contain the complex ion [Ni2(SrC4H 9)6]2_ (3), which is not only the first example of a tetrahedral nickel complex with alkane thiolate ligands, but also the first poly-nuclear nickel complex containing tetrahedral NiS4-units sharing a comm on edge. Reaction of nickel(II) chloride and sodium (2-trim ethylsilyl)thiophenolate in acetonitrile leads to [Ni(SC6H4SiM e3)4]2~ (5) with tetrahedral stereochemistry. The m ononuclear complex ion is isolated aso [Ph4P]2[Ni(SC6H4SiM e3)4]-5M eC N (4) with a = 13.771(2), b = 14.163(2), c = 25.873(4) A , a = 77.44(1), ß = 75.13(1), y = 72.46(1)°, space group P 1 and Z = 2. The final refinement converged to R = 0.0445. 
  Reference    Z. Naturforsch. 50b, 1464—1468 (1995); eingegangen am 29. Dezem ber 1994 
  Published    1995 
  Keywords    Ligands, Nickel Complexes, Synthesis, Crystal Structure, Bioinorganic Chemistry 
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 Identifier    ZNB-1995-50b-1464 
 Volume    50 
54Author    A. Franken, W. PreetzRequires cookie*
 Title    Darstellung, n B-NMR-und Schwingungsspektren  
 Abstract    von Am inohexahydro-closo-hexaborat(l-), [B6H6(NH2)]~ sowie Kristallstruktur von Cs[B6H6(NH2)]*H 20 P rep aratio n , n B N M R and V ibrational Spectra of A m in o h e x a h y d ro -c lo so -h ex a b o ra te (l-), [B6H 6(N H 2)]' , and the C rystal S tructure of Cs[B6H 6(N H 2)] • H 20 By reduction of [B6H5(N0 2)]2_ with Fe2+ in aqueous alkaline solution [B6H6(NH2)]~ is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] H20 has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) Ä, ß = 100.168(6)°. The UB NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N -H , B -H and B6 vibrations. 
  Reference    (Z. Naturforsch. 50b, 11—14 [1995]; eingegangen am 9. August 1994) 
  Published    1995 
  Keywords    Aminohexahydro-closo-hexaborate(l-), Crystal Structure, UB NMR Spectra, Vibrational Spectra 
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 Identifier    ZNB-1995-50b-0011 
 Volume    50 
55Author    Christian Drost, Carsten Jäger, Uwe Klingebiel, Christina Freire-Erdbrügger, Regine Herbst-Irm, M. Er, Artina SchäferRequires cookie*
 Title    Lithium-[N-di-terr-butylfluorsilyl-N' ,N ' -dimethyl-hydrazid] - Synthese, Kristallstruktur und Reaktivität Lithium (N-di-te/'f-butylfluorosilyl-N',N'-dimethyl)hydrazide - Synthesis, Crystal Structure and Reactivity  
 Abstract    Di-terf-butyldifluorosilane reacts with N-lithium -N',N'-dimethylhydrazine in a molar ratio 1:1 to yield the N-di-ferf-butylfluorosilyl-N',N'-dimethylhydrazine 1. The lithium derivative of 1 (2) forms a dimer with the nitrogen atoms coordinated "side-on" to the lithium atoms. The silylation with M e3SiCl gives product 3. Heating 2 in a vacuum leads to the cyclo-disilazane derivative 4. A bis(hydrazino)fluoroborane (5) is obtained in the reaction of 2 with trifluoroborane-etherate. 
  Reference    (Z. Naturforsch. 50b, 76—8 [1995]; eingegangen am 18. Juli 1994) 
  Published    1995 
  Keywords    Fluorosilylhyrazines, Lithium-Derivative, Crystal Structure, Side-on Coordination 
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 Identifier    ZNB-1995-50b-0076 
 Volume    50 
56Author    Evamarie Hey-Hawkins+, Stefan Kurz, G.Erhard BaumRequires cookie*
 Title    P-H-funktionelle Zirkonocen-Phosphido-Komplexe  
 Abstract    Synthese von Cp'2Zr{PH(2,4,6-Pr'3C6H2)}(X) (Cp = C5H4Me, X = Cl, 2,4,6-Pr'3C6H2) und Molekülstruktur von Cp'2ZrCl{PH(2,4,6-Pr/3C6H2)} P-H -Functionalized Zirconocene Phosphido Complexes -Synthesis of C p '2Zr{PH(2,4,6-Pr'3C6H 2)}(X) (Cp' = C5H 4 Me, X = Cl, 2,4,6-Pr'3C6H 2) and Molecular Structure of C p '2ZrCl{PH(2,4,6-Pr'3C6H 2)} The reaction of Cp'2ZrCl2 (Cp' = C5H4M e) with solvent-free LiPH(2,4,6-Pr'3C6H 2) yields the terminal zirconocene phosphido com plexes Cp'2ZrCl{PH(2,4,6-Pr'3C6H 2)} (1) (1:1 reac­ tion) or Cp'2Zr{PH(2,4,6-Pr'3C6H2)}2 (2) (1:2 reaction). 1 and 2 were characterized spectro­ scopically (NMR, IR, MS). An X-ray structure determination was carried out on 1 (Z r -P 2.6381(8) A, Z r-C l 2.4547(6) A , C l-Z r -P 93.55(2)°). 
  Reference    Z. Naturforsch. 50b, 239 (1995); eingegangen am 15. Septem ber 1994 
  Published    1995 
  Keywords    Zirconocene Phosphido Complexes, Lithium 2, 4, 6-Triisopropylphenylphosphide, Crystal Structure 
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 Identifier    ZNB-1995-50b-0239 
 Volume    50 
57Author    H. Szillat, Hk Müller-BuschbaumRequires cookie*
 Title    Uber das Erdalkalimetall-Lanthanoid  
 Abstract    Kupfer-Oxomolybdat (Cu0,22Mg0 ,78)BaNd2Mo4O 16 The Alkaline Earth R are E arth Copper-Oxomolybdate (C u 0 . 2 2 M g 0 . 7 8) B a N d 2 M o 4 O 1 6 Single crystals of (Cu0.22Mg0 78)B aN d2M o4O i6 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C ^ -C 1 2 /cl, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Ä, ß = 90.899(14)° and is isotypic to CuKHo2M o40 16. The crystal structure is dominated by B aO 10 and N d 0 8 poly-hedra forming a three-dimensional polyhedra network, which is filled by axially distorted (C u,M g)O fi octahedra and M o 0 4 tetrahedra. 
  Reference    Z. Naturforsch. 50b, 577 (1995); eingegangen am 4. Oktober 1994 
  Published    1995 
  Keywords    Crystal Structure, Copper, M agnesium, Barium, Neodymium, Molybdenum, Oxide 
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 Identifier    ZNB-1995-50b-0577 
 Volume    50 
58Author    Z. NaturforschRequires cookie*
 Title    Synthesis  
 Abstract    o f N itrene C om plexes w ith N -T rim ethylsilylaniline I. Characterisation and Crystal Structure o f [R e(N Ph)C l3(E t2PhP)2] and [Re(N Ph)Cl3(Ph3P)2] • 1/2CHC13 U rsula W ittern, Joachim Strähle*, U lrich A bram rra»^-mt'r-Trichlorobis(diethylphenylphosphine)phenylnitrene rhenium(V), [Re(NPh)Cl3-(Et2PhP)2], has been synthesized from [ReOCl3(Et2PhP)2] and N-trim ethylsilylaniline, while rrans-ttZfr-trichlorophenylnitrenebisCtriphenylphosphine) rhenium(V), [Re(NPh)Cl3(Ph3P)2] has been obtained via a novel route, from (Bu4N)[ReOCl4] and N-trim ethylsilylanilin. The products were studied by mass spectrometry, IR spectroscopy and X-ray diffraction. rrafls-m er-[Re(NPh)Ch(Et-'PhP)2] crystallizes in the m onoclinic space group P2i/n with a = 1498.5(3), b = 1068.6(1), c = 1784.0(4) pm and ß = 91.28(1)°, Z = 4. The rhenium atom exhibits a distorted octahedral coordination with the phosphine groups in trails positions, and the Cl ligands in a meridional arrangement. The R e = N -C moiety is linear with a bond angle o f 169,4(5)°and a R e = N bond length o f 171.8(6) pm. [ R e (N P h) C h (P h 3 P) i ] 0.5 C H C I 3 c r y s t a l l i z e s in th e t r i c l i n i c s p a c e g r o u p P i w i t h a = 1232.1 (4), b= 1431.6(5), c = 2236.6(8) pm, a = 89.19(2)°, ß = 80.50(2)°and 7 = 88.26(2)°, Z = 4. The asymmetric unit contains two symmetry independent complex m olecules o f approxima­ tely the same structure, with Cl atoms meridionally arranged and the phosphine groups in trans positions. The coordination geometry is a distorted octahedron. The almost linear R e = N -C m oieties have R e = N bond lengths o f 170.2(7) and 170.8(7) pm, respectively, and R e -N -C angles o f 173.3(6)°and 175.0(7)°. 
  Reference    Z. Naturforsch. 50b, 997 (1995); eingegangen am 15. Februar 1995 
  Published    1995 
  Keywords    Rhenium(V) C om plexes, Phenylnitrene Com plexes, Crystal Structure, Mass Spectra 
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 Identifier    ZNB-1995-50b-0997 
 Volume    50 
59Author    M. Jansen, S. StrojekRequires cookie*
 Title    Darstellung und Kristallstruktur von [P(C6H5)4]C13 Preparation and Crystal Structure of [P(C6H 5)4]C13  
 Abstract    Preparation and crystal structure of [P(C6H 5)4]C13 are reported. [P(C6H 5)4]C13 crystallizes in the monoclinic space group P 2 x!c with a = 1093.4(4), b = 789.1(1), c = 2682.7(7) pm, ß = 90.39(1)°, V = 2200.27-106 pm3, and Z = 4. The geometry of the trichloride anion in the solid state is almost linear (C1-C1-C1 = 178.44(4)°) and unsymmetrical (d (C l-C l) = 226.3(1) and 230.7(1) pm). 
  Reference    Z. Naturforsch. 50b, 1171—1174 (1995); eingegangen am 13. Februar 1995 
  Published    1995 
  Keywords    Tetraphenylphosphonium Trichloride, Preparation, Crystal Structure, G eom etry of Cl3~ 
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 Identifier    ZNB-1995-50b-1171 
 Volume    50 
60Author    Marcos Luján, Frank Kubel, Hans SchmidRequires cookie*
 Title    Crystal Growth, Room Temperature Crystal Structure and Phase Transitions of K M nP04  
 Abstract    Single crystals of K M nP 04 grown in a KC1 flux show ferroelastic domains. The structure was determ ined on an optically controlled single domain crystal by X-ray diffraction methods. The cell is triclinic with dimensions a = 5.4813(5), b = 8.627(1), c = 8.887(1), in A, a = 87.73(1)°, ß = 89.10(1)°, y = 88.01(1)°, VM = 419.6(1) A 3 and Z = 4. The structure is closely related to the stuffed /3-tridymite type. DTA experiments between room tem perature and 1000 °C and polarized light microscopy observations showed four phase transitions: at 165, 330, 353 and 707 °C. 
  Reference    Z. Naturforsch. 50b, 1210—1214 (1995); received February 20 1995 
  Published    1995 
  Keywords    Manganese Potassium Orthophosphate, Crystal Structure, Crystal Growth, Phase Transitions 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1210.pdf 
 Identifier    ZNB-1995-50b-1210 
 Volume    50 
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