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1Author    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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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1429.pdf 
 Identifier    ZNB-1995-50b-1429 
 Volume    50 
2Author    VeraV. Ponomareva3, VictorV. Skopenkoa, KonstantinV. Domasevitcha, Joachim Sielerb, Thomas GelbrichbRequires cookie*
 Title    Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}  
 Abstract    The caesium hydrogen benzoylcyanoximate (L_) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [mon­ oclinic, space group P2)/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Ä, ß = 90.13(1)°, V = 3434.3(9) Ä, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of C s(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}~, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O— O ca. 2.456(5)A], The caesium atom deviates by 1.492(3) A from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical "sunrise coordination" [C s-0 (ether) 3.040(9)-3.312(7) A], The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (C s-0 ca. 3.040(9), 3.312(7) A; Cs-N ca. 3.469(5), 3.679(6) A). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism. 
  Reference    Z. Naturforsch. 52b, 901—905 (1997); received February 28 1997 
  Published    1997 
  Keywords    Caesium Macrocyclic Complexes, Crown Ether Complexes, Benzoylcyanoxime, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0901.pdf 
 Identifier    ZNB-1997-52b-0901 
 Volume    52 
3Author    Joachim Pickardt, Pirka WischlinskiRequires cookie*
 Title    Kristallstruktur des "supramolekularen" Komplexes [K(Benzo-18-krone-6)][Zn(CN)3]*H20 mit einem polymeren kettenförmigen Tricyanozincat-Anion Crystal Structure of the "Supramolecular" Complex [K(benzo-18-crown-6)][Zn(CN)3] *H20 with a Polymeric Tricyano Zincate Anion with Chain Structure  
 Abstract    Crystals o f the com plex [K (benzo-18-crown-6][Zn(CN)3] H20 were obtained from a solution o f Z n(C N)2, KCN, and b en zo-18-crown-6 in water/methanol. The compound crystallizes in the triclinic space group PI (no. 2),: Z = 2, a = 818,6(5), b = 1236,7(8), c = 1359,6(6) pm, a = 67,02(4), ß = 87,38(4), 7 = 75,46(5). Each Zn atom is bonded to one bridging cyanide ion to give chains -Z n (C N)Z n -, and to two terminal CN groups. The N atom o f one o f the terminal CN groups interacts with a potassium ion o f the [K (benzo-18-crow n-6)]+ unit. The coordination spheres o f the K ions are completed by water molecules, which in turn form hydrogen bonds to N atoms o f terminal CN groups o f neighbouring chains, whereby puckered sheets are formed. 
  Reference    Z. Naturforsch. 54b, 747 (1999); eingegangen am 10. Februar 1999 
  Published    1999 
  Keywords    Zinc Cyanide C om plex, Crown Ether Complex, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0747.pdf 
 Identifier    ZNB-1999-54b-0747 
 Volume    54 
4Author    Michael Plate, Gerlinde Frenzen, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)l[SbCl6l und | V Cl(OH)( 18-Krone-6)(CH3CN)2] [SbCl6l * V2(18-Krone-6 * CH3CN) Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3( 15-Crown-5)(CH3CN)][SbCl6] and [VCl(OH)( 18-Crown-6)(CH3C N )2][SbCl6] ■ 'A( 18-Crown-6 * C H 3CN)  
 Abstract    The title compounds were prepared by the reaction o f titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction o f vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence o f traces o f water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations. [TiCl3(15-crown-5)(CH1CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflec­ tions, R = 0.035. Lattice dim ensions at -8 0 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The com pound consists o f SbCl6~ anions and cations [TiCl3(15-crown-5)(CH3C N)]+, in which the titanium atom is coordinated octahedrally by three chlorine atom s in facial arrangement, by the nitrogen atom o f the acetonitrile m olecule, and by two oxygen atom s o f the crown ether molecule. [VCl(OH)(18 -crown-6)(C H 3C N)2][SbCl6] ■ 'A(18-crow n-6 • C H 3 CN); Space group P I, 3936 observed unique reflections, R = 0.014. Lattice dim ensions at -8 0 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, « = 93.55(4)°, ß = 111.23(4)°, y = 93.15(4)°. The com pound con­ sists o f SbCl6-anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3C N)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms o f the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atom s o f the crown ether molecule. One o f the acetonitrile molecules forms weak hydrogen bridges with two oxygen atom s o f the includ­ ed crown ether molecule as well as with one chlorine atom o f the SbCl6" ion. 
  Reference    Z. Naturforsch. 48b, 149—155 (1993); eingegangen am 4. September 1992 
  Published    1993 
  Keywords    Crown Ether Complexes, Titanium, Vanadium, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0149.pdf 
 Identifier    ZNB-1993-48b-0149 
 Volume    48