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1994 (52)
21Author    Z. NaturforschRequires cookie*
 Title    Die isoelektronischen Molekülkomplexe TiCl3(NPPh3) und TiCl3(OSiPh3)  
 Abstract    The Isoelectronic M olecular C om plexes TiC l3(N P P h 3) and T iC l3(O SiPh3) Thilo R übenstahl, D o ro th ea W olff von G udenberg, F ra n k W eller, K u rt D ehnicke* TiCl3(NPPh3) and TiCl3(OSiPh3) have been prepared from titanium tetrachloride and Me3SiNPPh3 and HOSiPh3, respectively. Both complexes were characterized by IR spectrosco­ py and by crystal structure determmations. TiCl3(N PPhj): Space group R3, Z = 6, structure analysis with 959 observed unique reflec­ tions, R = 0.039. Lattice dimensions at -6 8 °C: a = b = 1370.5(7), c = 1845.9(9) pm. TiCl}(OSiPh3): Space group P2,/c, Z = 8, structure analysis with 4549 observed unique re­ flections, R = 0.049. Lattice dimensions at 19 °C: a = 2127.7(2), b = 947.2(1), c = 2136.8(1) pm, ß = 105.081(5)°. Both complexes form monomeric molecules in which the titanium atom is tetrahedrally coordinated by three chlorine atoms, the nitrogen atom of the phosphorone iminato ligand and the oxygen atom of the silyloxy group, respectively. The bond lengths TiN of 171.9(4) pm and TiO of 171.0(3) (in average) correspond to double bonds. 
  Reference    (Z. Naturforsch. 49b, 15—20 [1994]; eingegangen am 7. September 1993) 
  Published    1994 
  Keywords    Monomerie Titanium Complexes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0015 
 Volume    49 
22Author    Z. NaturforschRequires cookie*
 Title    Gold-Alkalimetallsysteme, III. Hochdrucksynthese und Kristallstruktur von Rb3Au7 [1]  
 Abstract    G old-A lkali M etal-System s, III. H igh Pressure Synthesis and C rystal S tructure o f R b 3A u 7 [1] K laus-Jürgen Range*, G eorg H. G rosch, F ran z R au, U lrich K lem ent The intermetallic compound Rb3Au7 could be synthesized from the elements at 4 kbar, 700 °C in a modified Belt-type apparatus. The structure (Cmmm; a = 5.579(1), b = 13.267(5), c = 7.265(2) Ä; Z = 2; R = 0.035, Rw = 0,031) comprises three crystallographically independ­ ent Au atoms, arranged in layers along the c-axis. The shortest interatomic distances are A u -A u = 2.633Ä, A u -R b = 3.438Ä and R b -R b = 3.622Ä. Im System R ubidium -G old [2,3] sind bisher n u r die V erbindungen R b A u [4] und R b A u 5 [5,6] ein­ deutig nachgewiesen und strukturell c h a ra k te ri­ siert w orden. Die Existenz von R b A u 2 [2,3,7] ko n n te bisher nicht verifiziert werden. D ie h o m o ­ logen V erbindungen N aA u 2 [8] und K A u 2 [9] sind Lavesphasen und kristallisieren im kubischen M gC u2-Typ bzw. im hexagonalen M g Z n 2-Typ. Bei unseren V ersuchen zur H ochdrucksynthese einer L avesphase R b A u 2 fanden wir nun eine bisher im System R b -A u unbekannte Phase d er Z u sam ­ m ensetzung R b 3A u 7, über die im folgenden berich­ tet w ird. 
  Reference    (Z. Naturforsch. 49b, 27—30 [1994]; eingegangen am 6. Juli 1993) 
  Published    1994 
  Keywords    Trirubidium Heptagold, High Pressure Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0027 
 Volume    49 
23Author    Wolfgang Blase, Gerhard Cordier, Matthias Ludwig, Rüdiger KniepRequires cookie*
 Title    Sr3[Al2N 4l: Ein Nitridoaluminat mit gewellten Tetraederketten * [AlN4/23 ] Sr3[Al2N 4]: A Nitridoaluminate with Corrugated Tetrahedral Chains j,[AlN4/23_]  
 Abstract    Sr3[Al2N 4] (Pnna, Nr. 52; a = 590.1(3), b = 1000.5(5), c = 958.0(4) pm; Z = 4) was prepared from the elements (m olar ratio Sr: A1 = 3:1; reaction with N 2, 1 atm, 24 h; Tmax = 1 1 0 0 °C). The crystal structure contains corrugated chains ifA lN ^ 3'] which consist of distorted A1N4 tetrahedra sharing com mon edges (A l-N : 188.5(7)-195.8(7) pm; N -A l-N : 95.0(3)-126.0(5)°). The nitrogen atom s form a distorted ccp arrangement. 3/4 of the octahedral holes are occupied by Sr atoms; 1 /4 o f the tetrahedral holes are occupied by A1 atoms. Sr3[Al2N4] can be described in terms o f the Zintl concept (isosteric relation of [AIN,]3-to SiS-,). 
  Reference    Z. Naturforsch. 49b, 501—505 (1994); eingegangen am 22. November 1993 
  Published    1994 
  Keywords    N itridoalum inate, Tetrahedral Chain-Anions, Preparation, Crystal Structure 
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 Identifier    ZNB-1994-49b-0501 
 Volume    49 
24Author    G. Tams, Hk Miiller-BuschbaumRequires cookie*
 Title    A Contribution to the Crystal Chemistry of Alcaline Alealine Earth Precious Metal Perovskites. Synthesis and Crystal Structure of NaBa4Cuo,5Pti,50 8  
 Abstract    Single crystals of the phase NaBa4Cu0 5P t1 s0 8 were prepared in closed silver tubes. The black and moisture sensitive crystals were investigated by four-circle diffractometer X-ray tech­ niques. They show trigonal symmetry, space group D2-P321, a = 10.0644, c = 8.3811 A, Z = 3 and belong to the perovskites. The typical M20 9 double octahedra are occupied by Pt4+ and Cu2+ in a different manner. Na+ is partly in and out of the centres of trigonal prisms of oxygen. These features will be discussed with respect 
  Reference    Z. Naturforsch. 49b, 585—588 (1994); eingegangen am 12. Januar 1994 
  Published    1994 
  Keywords    Sodium, Barium, Copper, Platinum, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0585.pdf 
 Identifier    ZNB-1994-49b-0585 
 Volume    49 
25Author    C. U., D. Osterloh, Hk Müller-BuschbaumRequires cookie*
 Title    Das erste Oxocuprat/-Arsenat mit Kupfer in gemischter Valenz  
 Abstract    ,56C u o , 4 4) C u (A s 0 4)3 The First O xocuprate/Arsenate Containing Mixed Valent Copper: Cu(Mg2.56Cu0.44)C u(A sO4) 3 Single crystals of Cu(Mg2 56Cu0 44)C u (A s0 4)3 have been prepared by C 0 2-LASER technique and investigated by X-ray diffraction methods. The light blue crystals show monoclinic sym­ metry, space group C2h-C 2/c, a = 11.897, b = 12.855, c -6.688 A, ß = 113.06°, Z = 4. The structure type is characterized by A s 0 4 tetrahedra, dumb-bell-like coordinated Cu(I), twisted C u 0 4 square polygons and octahedra statistically occupied by Mg/Cu2+. 
  Reference    Z. Naturforsch. 49b, 589—592 (1994); eingegangen am 14. Januar 1994 
  Published    1994 
  Keywords    Magnesium, Copper, Arsenic Oxide, Crystal Structure 
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 Identifier    ZNB-1994-49b-0589 
 Volume    49 
26Author    FrankW. Heinem, Helmut Hartung, NadjaM. Aier3, HermannM. Atschiner3Requires cookie*
 Title    Molekül-und Kristallstruktur der Verbindung 8-(n-Butylamino- phenyl-methyliden)  
 Abstract    -l,2,3?4,5,6,7-heptathiocan Molecular and Crystal Structure of 8-(«-Butylamino-phenyl-methylidene)-l,2,3,4,5,6,7-heptathiocane By the reaction of acetophenone with sulfur and primary amines yellow-coloured crystals of the title compound are formed. It crystallizes in the monoclinic space group P 2 x!n with lattice constants a = 1309.9(2) pm, b = 926.5(2) pm, c -1582.2(2) pm and ß -114.00(1)°. The structure of the eight-membered heptathiocane ring is characterized by a crown confor­ mation. The range of the S -S distances [204.4(1)-207.3(1) pm], the S -S -S bond angles [107.2(1) — 109.0(1)°] and the S-S-S-S torsion angles [93.2(1)-97.7(1)°] is comparable to those observed in a-, ß-and y-sulfur. 
  Reference    Z. Naturforsch. 49b, 1063—1066 (1994); eingegangen am 3. Februar 1994 
  Published    1994 
  Keywords    Heptathiocane, Acetophenone, Sulfur, Crystal Structure, Crown Conformation 
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 Identifier    ZNB-1994-49b-1063 
 Volume    49 
27Author    Rainer Pöttgen, G. Ünter Block, Wolfgang Jeitschko, RonaldK. BehrensRequires cookie*
 Title    Preparation and Crystal Structure of the Carbides Ln12Re5C15 (Ln = Y, L a-N d, G d-E r)  
 Abstract    The title compounds were prepared by arc-melting of the elem ental components and sub­ sequent annealing. Their crystal structure is hexagonal P 6 2 m with one formula unit per cell. It was determined from single-crystal X-ray data o f La12R e5C i5 (a = 1116.8(1) pm. c = 545.3(1) pm. R = 0.060 for 287 structure factors and 27 variable parameters) and H o 12R e5C i5 (a = 1066.7(1) pm, c -504.2(1) pm, R = 0.018 for 392 F's and 31 variables). The structures correspond to the formula Ln12[ReC 3]2[R e3C3(C2)3], where the brackets indicate two differ­ ent trigonal planar anionic rhenium-carbon groups. The coordination of the rhenium atoms in these polyanions seem s to be compatible with the 18-electron rule. 
  Reference    Z. Naturforsch. 49b, 1081—1088 (1994); received February 22 1994 
  Published    1994 
  Keywords    Crystal Structure, Lanthanoid-Rhenium-Carbides, 18-Electron Rule 
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 Identifier    ZNB-1994-49b-1081 
 Volume    49 
28Author    YueQing Zheng, Arnold AdamRequires cookie*
 Title    Ein neues Carbonat mit Baylissit-Struktur: Rb2[M g(C 03)2(H 20 )4] A New Carbonate with Baylissite Structure: Rb2 [Mg(C0 3 )2(H 2 0 )4]  
 Abstract    The new complex carbonate Rb2[M g (C 0 3)2(HoC))4] crystallizes in the Baylissite-tvpe structure with a = 1130,4(3), b = 641,9(1), c = 703,3(2) pm, ß = 99,62(1)°, V EZ = 503,2(2), space group P2l/n (No. 14) and Z = 2. In comparison with the isostructural potassium compound the cell dimensions increase in b-and c-and decrease in ö-direction. This effect depends on the greater coordination number of Rb+ and the rigidity of strong hydrogen bonds. The carbonate anion exhibits significant deviations from D 3h-symmetry (C -O : 127,1(5)-130,2(5) pm, Z_ O -C -O : 117.9(4)-121,1(3)°). 
  Reference    Z. Naturforsch. 49b, 1368—1372 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    M etal-Carbonato-Complex, Baylissite Type, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-1368 
 Volume    49 
29Author    Stefan Peschel, Dietrich BabelRequires cookie*
 Title    Zur Kristallstruktur der Cyanoelpasolithe [N(CH3)4]2CsCo(CN)6 und [H3NCH3]2NaFe(CN)6 Concerning the Crystal Structures of the Cyano-Elpasolites [N(CH3 )4]2CsCo(CN) 6 and [H3NCH3]2NaFe(CN) 6  
 Abstract    Single crystals of the cyano com plexes [N (C H 3)4]2C sC o(C N)6 and [H3NCH 3]2N aFe(C N)6 were prepared and their structures determined by X-ray methods. The cobalt compound is monoclinic, a -885.5(1), b = 892.6(2), c = 1259.9(5) pm, ß = 90.29(4)°, space group 12Im, Z = 2; R l = 0.048 for 861 independent reflections. The resulting average distances in the nearly undistorted octahedra are C o -C = 189.8, C -N = 114.1, C s -N = 325.6 pm. The iron compound exhibits a cubic elpasolite type structure, a = 1105.2(1) pm, space group Fm 3m , Z = 4; R l = 0.040 for 127 independent reflections; F e -C = 193.4(6), N a -N = 247.7(8) pm. The orientation of the librating tetramethyl-ammonium group within the cages of the cobalt compound and the disorder of the monomethyl-ammonium cation around the special site (1/4, 1/4, 1/4) of the iron complex are discussed. 
  Reference    Z. Naturforsch. 49b, 1373—1380 (1994); eingegangen am 31. März 1994 
  Published    1994 
  Keywords    Hexacyanometallates(III), Crystal Structure, Elpasolite 
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 Identifier    ZNB-1994-49b-1373 
 Volume    49 
30Author    M. Arkus Wieber, Stefan Lang, StefanRalph Rohse, Christian Habersack, BurschkaRequires cookie*
 Title    Synthese und Kristallstruktur von Triphenyltelluroniumsulfid Synthesis and Crystal Structure of Triphenyltelluroniumsulfide  
 Abstract    The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P I) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, a = 77.67(3)°, ß = 82.18(2)°, y = 66.00(2)° (V = 1766(1) x 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two m ole­ cules of CH2C12 per unit cell. 
  Reference    Z. Naturforsch. 49b, 1654—1658 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Triphenyltelluroniumsulfide, Synthesis, NMR Data, Crystal Structure, Secondary Bonding 
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 Identifier    ZNB-1994-49b-1654 
 Volume    49 
31Author    JonesRequires cookie*
 Title    Polysulfonylamine  
 Abstract    , LIV [1] (12-Krone-4)lithiumdimesylamid-Acetonitril (3/2): Ein Kristall mit zwei prinzipiell unterschiedlichen Konformationen des gleichen Coronanden Polysulfonylam ines, L IV [1] (12-Crow n-4)lithium D im esylam ide-A cetonitrile (3/2): A Crystal w ith Two F undam entally D ifferent C onform ations of the Sam e C oronand A rm an d Blaschette*, K arl-H einz N agel, P e te r G. [Li(12-crown-4){N(S02CH3)2}] is obtained from equimolar amounts of lithium dimesyl­ amide and 12-crown-4 in methanol and crystallizes from acetonitrile as a 3/2 solvate. The crystallographic data of the latter at -130 °C are: monoclinic, space group P 2In, a = 1053.4(3), b = 904.3(3), c = 2791.2(8) pm, ß = 95.66(3)°, V = 2.646 nm3, Z = 6, Dx = 1.441 Mgm~3. Apart from CH3CN molecules residing in lattice cavities, the structure consists of two crystallogra-phically independent [Li(12-crown-4){N(S02CH3)2}] ion pairs A and B in the ratio 2:1. In B, the Li and N atoms lie on a crystallographic twofold axis. In both ion pairs, Li is hexa-coordinated by the four crown oxygen atoms O(C) and by one oxygen O(S) from each sul-fonyl group of the anionic ligand. The coordination geometry of Li in A closely resembles that of Cu11 in the known structure of [Cu(12-crown-4)Cl2] and can be pictured as a distorted octahedron, where two cis sites are occupied by the O(S) atoms and the remaining vertices by the four oxygens of the macrocycle, which displays a [4 8] conformation. The lithium atom, the two O(S) and two O(C) atoms are arranged in an approximately square-planar pattern with L i-O (S) 203.6 and 205.1, L i-O (C) 206.9 and 219.1 pm, trans angles of 173.7 and 174.8°, and cis angles in the range 87.1 -93.6°. The angle between the remaining two Li -O(C) bonds with distances 214.7 and 221.5 pm is only 146.5° compared with 180° in an ideal octahedron. In ion pair B, the coronand assumes a [3 3 3 3] conformation close to C4 symmetry, as observ­ ed e. g. in the known structures of [Li(12-crown-4)NCS] with a square-pyramidal 0 4N-co-ordination and [Ca(12-crown-4)(H20) 4]Cl2-4 H zO with a square-antiprismatic 0 8-geometry. The coordination polyhedron in B can be viewed as an incomplete cube in which two verti­ ces related by a face diagonal are unoccupied. Important bond lengths and angles in B are: L i-O (S) 216.8, L i-O (C) 214.0 and 228.7pm; 0 (S) -L i-0 (S) 82.0, 0 (C) -L i-0 (C) 75.7/76.3 for adjacent and 120.4/121.9° for opposite ring oxygens. 
  Reference    (Z. Naturforsch. 49b, 36—42 [1994]; eingegangen am 2. September 1993) 
  Published    1994 
  Keywords    Polysulfonylamines, (12-Crown-4)lithium Dimesylamide, Synthesis, Crystal Structure, Coronand Conformation 
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 Identifier    ZNB-1994-49b-0036 
 Volume    49 
32Author    Anne-Kathrin Duhme, Henry StrasdeitRequires cookie*
 Title    Ligandenmangelkomplexe des Cadmiums. Synthese und spektroskopische Charakterisierung molekularer (Pentafluorphenyl)cadmium-Thiolate und die Struktur des Cubankomplexes [{Cd(C6F5)(SBur)}4] Ligand-Deficient Complexes of Cadmium. Synthesis and Spectroscopic Characterization o f Molecular Pentafluorophenyl Cadmium Thiolates and the Structure o f the Cubane Complex [{Cd(C6F5)(SBuf)}4]  
 Abstract    In toluene, bis(pentafluorophenyl)cadmium(II) and thiols RSH (R = Bu', 2,4,6-Pr'3C6H2, 2,4,6-Bu'3C6H2) react to give soluble pentafluorophenyl cadmium thiolates [(Cd(C6F5)(SR)} J. The compounds [{Cd(C6F 5)(SBu')}4] (1)0 .5 C6H5CH3, [ {Cd(C6F5)(SC6H2Pr'3-2,4,6)} J (2)-ca. 0.25n C6H 5CH3, and [{Cd(C6F5)(SC6H2Bu'3-2,4,6)} J (3) ca. 0.25« C6H5CH3 have been prepared in 65, 59 and 78% yield, respectively. 1-0.5 C6H5CH3 crystallizes in the triclinic space group PI with a = 11,635(1)Ä, b = 11.583(1)Ä, c = 21.480(2)Ä, a = 82.12(1)°, ß = 76.26(1)°, y — 89.35(1)°, and Z = 2. 1 is a cubane-type complex with a {Cd4(/z3-SBur)4}4+ core. Each Cd atom is coordinated by three bridging thiolato ligands and one terminal C6F5 group (C d -S 2.62 A, C d -C 2.15Ä (mean values)). The central C atoms of the Bu'S" ligands of 1 show a remarkable low-field shift o f their 13C N M R resonance (12.3 ppm relative to the value of the free thiol). A characteristic spectral feature of (Cd(C6F5) } + complexes is the large value of the coupling constant 2/ (19F ,13C) o f the ipso-C atom (1, 2: 68 Hz; 3: 67 Hz). The complexes [Cd(C6F5)(SR) + H]+, [Cd(SR)2 + H]+, and [Cd2(SR)3]+ were identified in the Cl mass spectra (/50-butane) of 2 and 3. 
  Reference    (Z. Naturforsch. 49b, 119—127 [1994]; eingegangen am 17. August 1993) 
  Published    1994 
  Keywords    Cadmium Complexes, Thiolates, Crystal Structure, NMR Spectra, Mass Spectra 
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 Identifier    ZNB-1994-49b-0119 
 Volume    49 
33Author    Dietrich Mootz, Michael BornRequires cookie*
 Title    Niedere Hydrate von Aminen. Kristallstrukturen der Hemihydrate von Ethyl-und Diethylamin sowie des Hemi-und Monohydrats von 1-Butylamin [1] Lower Hydrates of Amines. Crystal Structures of the Hemihydrates of Ethyl-and Diethylamine and the Hemi-and M onohydrate of 1-Butylamine  
 Abstract    The melting diagrams of three systems alkylamine-water have been reexamined and the crystal structures of four lower hydrates determined for the first time. The hydrate EtNH2 -0.5 H20 , m.p. -72 °C, is triclinic with space^roup P 1 and Z = 4 formula units per unit cell of dimensions a = 5.104, b = 8.137, c = 9.394 Ä, a = 100.41, ß = 98.41 and y = 97.96° at -150°C. The O and N atoms are hydrogen-bonded into a two-dimensional array l[ON6/3] analogous to the layer of the Cdl2 structure type. The hydrate Et2NH • 0.5 H20 , m.p. -20 °C, is monoclinic with 12/a, Z = 8 , a -8.324, b = 15.090, c = 10.006 Ä and ß -103.34° at -100 °C. The O and N atoms are linked into a four-membered ring spiro chain ifON^] analogous to that in SiS2. The hydrate l-BuNH2 0.5H20 (m.p. -57 °C, monoclinic, P 2x/c, Z = 8,a = 14.994, b = 5.086, c = 16.15 A .,ß -103.45° at -81 °C) contains essentially the same hydrogen-bonded array as the hydrate EtNH,-0.5H20 (see above). l-BuNH2-H20 , the only monohydrate in­ vestigated besides the three hemihydrates (m.p. -60 °C, monoclinic, C 2/m, Z = 4, a = 9.68, b = 4.238, c = 15.58 A, ß = 94.9° at -81 °C), has also a two-dimensional H20/N H 2 partial structure, similar to a subset of the three-dimensional network of the adduct NH3 H20 of analogous composition. Z ur Bildung kristalliner Hydrate von einfachen Alkylaminen gibt es eine Reihe von z. T. schon recht frühen Untersuchungen mit allerdings nicht immer eindeutigen und widerspruchsfreien Ergebnissen. Die Bestimmung von Kristallstrukturen be­ schränkte sich bisher auf einige höhere Hydrate mit W assergehalten oberhalb denen von Pentahydra-ten. Solche wasserreichen Phasen wurden als Cla-thrathydrate oder Semiclathrate charakterisiert. Sie enthalten nämlich dreidimensional vernetzte W irtsstrukturen aus den W assermolekülen und in deren m ehr oder weniger gestörten polyedrischen H ohlräum en die fast immer auch noch H-brücken-aktiven (N -H — O und/oder O -H -N) Am in­ moleküle als Gastspezies [2]. Gegenstand der vorliegenden A rbeit sind nun erstmals K ristallstrukturen niederer Hydrate von * Sonderdruckanforderungen an Prof. Dr. D. Mootz. 
  Reference    Z. Naturforsch. 49b, 243—249 (1994); eingegangen am 27. Oktober 1993 
  Published    1994 
  Keywords    Amine Hydrates, Lower Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding 
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 Identifier    ZNB-1994-49b-0243 
 Volume    49 
34Author    P. Souza, M. A. Mendiola3, A. Arquerob, V. Ferná, E. G Utiérrez-Pueblac, C. Ruiz-ValerocRequires cookie*
 Title    Copper(II) Complexes of Hydrazone Derivatives  
 Abstract    Three benzil based, macrocyclic oxygen-, nitrogen-, and sulfur-containing ligands, (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7,14-dithione-2,4,9,11 -tetraene) ethanol (L 1), 10,1 l-diethoxy-3,4,10,11-tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dithione-2,4-diene (L2), (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dione-2,4,9,l 1-tetraene) ethanol (L3); a cyclic ligand, 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L5) and two open chain ligands, benzilsemicarbazone (L6) and benzilbisthiosemicarbazone (L4) are reported. These ligands react with copper(II) chlor­ ide, nitrate and acetate. The complexes obtained have been characterized on the basis o f N M R , IR, electronic and mass spectral studies, conductance and analytical data. The sto-ichiometry and the spectroscopic data o f the complexes indicate that the copper ions are coor­ dinated by neutral ligands or by ligand anions formed by loss o f protons from the ligand. The molecular and crystal structure o f 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L 5) was determined by X-ray diffraction; the space group is triclinic, P 1 with a = 7.865(1), b = 14.101(6), c = 15.733(9) A, a = 69.10(3)°, ß = 75.62(2)°, y = 86.69(2)°, V = 1578(1) A 3, Z = 4. 
  Reference    Z. Naturforsch. 49b, 263—2 (1994); received June 2/October 4 1993 
  Published    1994 
  Keywords    Benzil, Hydrazones, Copper(II), M acroligands, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0263.pdf 
 Identifier    ZNB-1994-49b-0263 
 Volume    49 
35Author    Meyer Zu Köcker, Andreas Behrendt, K. Urt Dehnicke, Dieter FenskeRequires cookie*
 Title    Phosphaniminato-Cluster des  
 Abstract    Kupfers. Synthese und Kristallstrukturen von ICu6Cl6(NPM e3)4|Cl[Me3SiNPM e3| • CH2C12 und ICu6Cl6(NPM e3)4l[Cu(Me3SiNPM e3)2lCl2 Phosphoraneim inato Clusters o f Copper. Syntheses and Crystal Structures of [Cu6Cl6(N PM e3)4]Cl[Me3SiNPM e3] • C H 2C12 and [Cu6Cl6(NPM e3)4][Cu(Me3SiNPM e3)2]Cl2 R olf The title com pounds have been prepared as black-blue crystals with metallic lustre by the reaction o f CuCl2 and CuCl, respectively, with M e3SiN P M e3 in C H 2C12 suspensions. The com ­ plexes have been characterized by cyclic voltammetry and by crystal structure determinations. [Cu6Cl6(N P M e3)4]Cl[M e3SiN P M e3] • C H 2C12: Space group P 2,2,2,, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -7 0 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, in which the copper atom s form a regular octahedron. Four planes o f the octahedra are capped by //3-nitrogen atom s o f the (N P M e3)~ groups. Each o f the Cu atom s is connected with a terminal chlorine atom . Another chloride ion serves for charge com pensa­ tion; this ion occupies another Cu3 plane o f the octahedron. W ithout bonding interaction one M e3SiN P M e3 molecule and one C H 2C12 molecule are included in the lattice. [Cu6Cl6(N P M e3)4][Cu(M e3SiN P M e3)2]Cl2: Space group Pna2,, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -7 0 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, the com plex ion [Cu(M e3SiN PM e3)2]+, and chloride ions. In the cation [Cu(Me3SiN P M e3)2]+ the copper atom is linearly coordinated by the nitrogen atom s o f the phosphaneimine m olecules. 
  Reference    Z. Naturforsch. 49b, 301—3 (1994); eingegangen am 18. November 1993 
  Published    1994 
  Keywords    Phosphoraneim inato Clusters o f Copper, Synthesis, Cyclic Voltammetry, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0301.pdf 
 Identifier    ZNB-1994-49b-0301 
 Volume    49 
36Author    Holger Szillat, Hanskarl Müller-BuschbaumRequires cookie*
 Title    Synthese und Kristallstruktur von KCuHo2Mo40 16 Synthesis and Crystal Structure of K C uH o2M o40 I6  
 Abstract    Single crystals o f K C uH o2M o40 16 have been prepared by recrystallisation from melts and investigated by X-ray diffractometer techniques. The compound crystallizes with m onoclinic symmetry, space group C 2/c, a = 521.6(1), b = 1251.3(2), c = 1953.1(2) pm, ß = 92.903(18)°, Z -4. K C uH o2M o40 16 represents a new structure type characterized by H oO s and alternate CuO6/K O 10 polyhedra chains. The connection o f these polyhedra chains to each other and by M o 0 4 tetrahedra is described and the crystal structure discussed with respect to related com ­ pounds o f the C uLnM o2Os and K L nM o20 8 types. 
  Reference    Z. Naturforsch. 49b, 350 (1994); eingegangen am 10. Dezember 1993 
  Published    1994 
  Keywords    Crystal Structure, Copper, H olm ium, M olybdenum, Potassium 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0350.pdf 
 Identifier    ZNB-1994-49b-0350 
 Volume    49 
37Author    Mitra Ghassemzadeh, Kurt Dehnicke, Helmut Goesmann, Dieter FenskeRequires cookie*
 Title    //2-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh4[X(N-Iodsuccinimid)2] * CH3CN mit X = Cl, Br, I /^2-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh4 [X(N-Iodosuccinimide)2] * CH 3CN with X = Cl, Br, I  
 Abstract    The ,a2-halogeno complexes PPh4[X(N-Iodosuccinimide)2] • CH 3CN with X = Cl. Br, I have been prepared by reactions of N-Iodosuccinimide with the corresponding tetraphenylphos-phonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determina­ tions. PPh4[Cl(N-Iodosuccinimide)2] C H 3CN (1): Space group Pna2!, Z = 4, 4461 observed unique reflections, R -0.027. Lattice dimensions at -6 0 °C: a = 1840.5(9), b = 2589(1), c = 728.2(4) pm. 
  Reference    Z. Naturforsch. 49b, 602—608 (1994); eingegangen am 22. Dezember 1993 
  Published    1994 
  Keywords    Halogeno Complexes of N-Iodosuccinimide, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0602.pdf 
 Identifier    ZNB-1994-49b-0602 
 Volume    49 
38Author    M. Ahm, Shakibaie-M Oghadam, Ulrich Timper, Gert HellerRequires cookie*
 Title    Darstellung und Struktur dreier verschiedener Bis(ethylendiamin)-kupfer(II)-tetraborate Preparation and Structure o f Three Different Bis(ethylenediamine) Copper(II) Tetraborates  
 Abstract    Three different bis(ethylenediamine) Copper(II) tetraborates have been prepared: Cu(en),[B40 5(0 H)4]-2 B (0 H)3 (A), 2{Cu(en),B (0H)3 H 20[B 40 5(0 H)4]} H ,0 (B) and 
  Reference    Z. Naturforsch. 49b, 627—634 (1994) 
  Published    1994 
  Keywords    Bis(ethylenediamino) Copper Tetraborates, Boric Acid Molecules, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0627.pdf 
 Identifier    ZNB-1994-49b-0627 
 Volume    49 
39Author    IrinaB. Ecker, M. Arcus, W. Indhaus, R. Ainer, M. AttesRequires cookie*
 Title    Synthesen, 121Sb-Mößbauer-Spektren und  
 Abstract    Strukturen von [SbF3(18-Krone-6)], [SbF3(18-Krone-6)]*CH3CN und [(SbF3)2(12-Krone-4)] Synthesis, 121Sb-M ößbauer Spectra and S tructures of [SbF3(18-Crown-6)], [SbF3(18-Crown-6)] C H 3CN, and [(SbF3)2(12-Crow n-4)] The crown ether complexes SbF3(18-crown-6) (1), SbF3(18-crown-6) • CH3CN (2) and (SbF3)2(12-crown-4) (3), have been prepared by reactions of SbF3 and the corresponding crown ether. They have been characterized by IR. Raman and 121Sb-Mößbauer spectroscopy, and by X-ray structure determinations. The s electron density at the Sb atom is diminished in these complexes. 1 and 2 show a symmetrical half-sandwich structure, with coplanar O atoms and S b -O distances ranging from 298 to 321 pm. 3 has a band-like structure. The two metal centers adopt different stereochemistries. The S b -O distances are in the range from 269 to 325 pm. One oxygen atom of 12-crown-4 has a bridging function. Crystal data for 1: space group P 21212i, a = 823,1(1), b = 1146,1(2), c = 1807,0(3) pm, Z = 4; 2: space group P2,/c. a = 1257,7(3), b = 828,9(2), c -1895,5(5) pm, ß = 93,68(2). Z = 4; 3: space group P2j/c, a = 805,6(1), b = 2143,1(4), c = 836,4(2) pm, ß = 90,98(1), Z = 4. 
  Reference    Z. Naturforsch. 49b, 870—876 (1994); eingegangen am 30. Dezember 1993 
  Published    1994 
  Keywords    Crown Ether Complexes of SbF3, 121Sb-Mößbauer Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0870.pdf 
 Identifier    ZNB-1994-49b-0870 
 Volume    49 
40Author    Birgit Bäck, H. An, S. PreutRequires cookie*
 Title    Uber die Reaktionen von Molekülen  
 Abstract    (R2CS)2 (R = CF3, CI) und C12CS mit XeF+MF6-(M = As, Sb) und Kristallstruktur von (CF3)2CSC(CF3)2SF+SbF6-[1] O n th e R eactions of M olecules (R 2C S)2 (R = C F 3, Cl) and C12CS with X eF +M F6_ (M = As, Sb) and C rystal Structure of (C F3)2C SC (C F3)2SF+SbF6~ [1] R olf M inkwitz XeF+MF6_ (M = As, Sb) reacts with ((CF3)2CS)2 and C12CS to form the corresponding monofluorinated sulfonium hexafluorometalates. The salts have been characterized by vibra­ tional and 19F NMR spectroscopic measurements. (CF3)2CSC(CF3)2SF+SbF6^ crystallizes in the monoclinic space group C2/c with a =o 14.791(10), b = 11.093(6), c -10.356(6)Ä, ß -119.83° and Z = 4. With a value of 1.51(1) A d (S -F) is comparable to the SF-bond distance in (CF3)(C1)CSC(CF3)(C1)SF+AsF6-. 
  Reference    Z. Naturforsch. 49b, 881—888 (1994); eingegangen am 10. November 1993 
  Published    1994 
  Keywords    Monofluorosulfonium Salts, Preparation, Vibrational Spectra, 19F NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0881.pdf 
 Identifier    ZNB-1994-49b-0881 
 Volume    49 
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