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161Author    Z. NaturforschRequires cookie*
 Title    Lanthanoiden-Komplexe, IX [1]  
 Abstract    Reaktivitätsbestimmender Einfluß der Ligandenkonstitution bei Seltenerdamiden: Herstellung und Struktur sterisch überladener Alkoxid-Komplexe L anthanoid Com plexes, IX [1] Reactivity C ontrol o f L an th an o id A m ides through Ligand Effects: Synthesis and S tructures of Sterically C ongested Alkoxy Com plexes W olfgang A. H errm an n * , R ein er A nw ander, Florian C. M unck, W olfgang Scherer, V eronique D u fau d 3, N o rb ert W. H u b e rb, G eorg R. J. A rtus It is shown that the introduction o f sterically demanding ligands in lanthanoid metal com ­ plexes can depend more on the precise composition of the lanthanoid precursor than on the size of the new ligand. Thus, tris(r-butyl)methanol ("tritox-H ") does not react with the amides Ln[N(SiM e3) 2 ] 3 of the "late" (small) lanthanoid metals. However, fast and clean reactions occur with the sterically less demanding derivatives Ln[N(SiHM e2)2]3, with new homoleptic com plexes Ln(tritox)3 (Ln = Y, Nd) being formed with practically all metals o f this group of elements. The molecular and crystal structures of some lanthanoid amides and alkoxides are described. 
  Reference    Z. Naturforsch. 49b, 1789—1797 (1994); eingegangen am 30. März 1994 
  Published    1994 
  Keywords    Lanthanoid Complexes, Alkoxides, Amides, Synthesis, Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1789.pdf 
 Identifier    ZNB-1994-49b-1789 
 Volume    49 
162Author    H. Vogt, C. Frauendorf, A. Fischer, P. G. JonesRequires cookie*
 Title    Synthese und Kristallstruktur von Tribrommethyltriphenylphosphonium-bromid und Bis(tribrommethyltriphenylphosphonium)-tribroniid-bromid Synthesis and Crystal Structure of Tribrom om ethyltriphenylphosphonium Bromide and Bis(tribrom omethyltriphenylphosphonium ) Tribromide Bromide  
 Abstract    Tribromotriphenylphosphonium bromide 1 has been prepared by the reaction o f triphenyl-phosphine with tetrabromomethane in dichloromethane. Colourless crystals were obtained by recrystallization from the same solvent. The^ light-sensitive crystals change colour to yel­ 
  Reference    Z. Naturforsch. 50b, 223 (1995); eingegangen am 28. Septem ber 1994 
  Published    1995 
  Keywords    Tribromomethyltriphenylphosphonium Bromide, Bis(tribromomethyltriphenylphosphonium) Tribromide Bromide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0223.pdf 
 Identifier    ZNB-1995-50b-0223 
 Volume    50 
163Author    JanKarsten Schaefer, BluhmRequires cookie*
 Title     
 Abstract    uT m 2[ B 20 5] 2: D as erste "M etaborat" mit einem x [ B 20 5] 4 -Anion CuTm2[B20 5]2: The First " Metaborate" with a ^ [ B ^ s ] 4 -Anion Single crystals o f the compound CuTm2[B 20 3]2 were obtained by a B20 3 flux technique. The compound contains a hitherto unknown metaborate anion with the formula ^ [ ^ O s ] 4-. It crystallizes in the monoclinic space group C|h-P2!/c with a = 452.18(7); b = 720.0(2); c = 929.2(5) pm; ß -90.16(5)°; Z = 2. The metaborate layers consists of four and eight membered rings of edge-sharing B 0 4-tetrahedra resembling the complex anion in the isotypic gadolinite structure of F e Y 2[B eS i0 3]2. The layers are connected via copper-centered elongated oxygen octahedra and slightly distorted thulium-centered tetragonal oxygen antiprisms. 
  Reference    Z. Naturforsch. 50b, 630—634 (1995); eingegangen am 2. August/11. November 1994 
  Published    1995 
  Keywords    Copper, Thulium, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0630.pdf 
 Identifier    ZNB-1995-50b-0630 
 Volume    50 
164Author    Wilfried Bubenheim, Ulrich MüllerRequires cookie*
 Title    Tetraphenylphosphonium- tris(tetrasulfido)stannat, (PPh4)2[Sn(S4)3] Tetraphenylphosphonium Tris-tetrasulfido- stannate, (PPh4)2[Sn(S4)3]  
 Abstract    PPh4[SnCl3] reacts with Na2S4 in acetonitrile to give the title compound as one of the products. Its crystal structure was determined by X-ray diffrac­ tion (R = 0.071 for 3288 reflexions). Crystal data: monoclinic, P2JC, Z = 4, a = 1301.2(3), b = 1139.1(2), c = 3476.2(7) pm, ß = 97.82(3)°. (PPh4)2[Sn(S4)3] is isotypic with (PPh4)2[Sn(Se4)3] and contains [Sn(S4)3]2-ions in which three tetra-sulfido groups are chelating an octahedrally coordi­ nated tin atom. 
  Reference    Z. Naturforsch. 50b, 1135 (1995); eingegangen am 27. Januar 1995 
  Published    1995 
  Keywords    Tetraphenylphosphonium tris-tetrasulfido-stannate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1135_n.pdf 
 Identifier    ZNB-1995-50b-1135_n 
 Volume    50 
165Author    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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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1377.pdf 
 Identifier    ZNB-1995-50b-1377 
 Volume    50 
166Author    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 
167Author    Ute Berger, Wolfgang SchnickRequires cookie*
 Title    Ba2Na(CN2)(CN)3, ein neues Cyanamid-cyanid mit interpenetrierenden Teilstrukturen Ba2Na(CN2)(CN)3, a Novel Cyanamide Cyanide with Interpenetrating Substructures  
 Abstract    Ba2Na(CN2)(CN)3 was obtained by the reaction of Ba2N with melamine and NaCN at 700 °C. The compound was structurally characterized by single-crystal X-ray investigations (Fd3m, a = 1518.8(3) pm, Z = 16). In the crystal structure the Ba"+ ions form a cubic close packed arrangement, the Na+ and the CN2_ ions occupy the octahedral interstices. The CN-ions are located within the close packed Ba2+ layers. The unit cell of Ba2Na(CN2)(CN)3 contains two interpenetrating substructures of the zinc-blende structure type, building up a variant of NaTl. A reversible phase transition has been observed during cooling of the compound. Whereas the Ba2(CN2)(CN)3 sublattice remains nearly unaffected in this process, the Na+ ions of the low-temperature phase are statistically distributed on two crystallographic positions. 
  Reference    (Z. Naturforsch. 51b, 1—8 [1996]; eingegangen am 7. Juni 1995) 
  Published    1996 
  Keywords    Cyanamide Cyanides, Synthesis, Crystal Structure, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0001.pdf 
 Identifier    ZNB-1996-51b-0001 
 Volume    51 
168Author    E. Kemnitz3, C. Werner3, A. Stiewe3, H. Worzalab, S. Trojanov3Requires cookie*
 Title    Synthese und Struktur von Zn(HS0 4)2(H2S0 4)2 und Cd(H S04)2 Synthesis and Structure of Z n(H S04)2(H2S 0 4)2 and C d(H S 04)2  
 Abstract    From the binary systems M2S 0 4/H2S 0 4 (M = Zn, Cd), two new hydrogen sulfates, (Zn(HS0 4)2(H2S04)2 and Cd(HS04)2, have been synthesized and structurally characteri­ zed. Both compounds crystallize in the monoclinic space group P2,/c with cell parameters a = 5.047(2), b = 15.430(4), c = 7.958(3) A and ß = 104.16(4)° (Z= 2) for Zn(HS04)2(H2S 0 4)2 and a = 5.339(1), b = 13.351(3), c = 8.508(2) A and ß = 92.22(3)° (Z = 4) for Cd(H S04)2. In the zinc compound there are slightly distorted centrosymmetric Z n 06 octahedra with Z n -0 distances of 2.05 -2.13 A which are sharing corners with S 0 4 tetrahedra. H S 04 and H2S 0 4 tetrahedra are linked via hydrogen bonds to form layers perpendicular to the c-axis. In the crystal structure of C d(HS04)2there exist two crystallographically different H S 04 tetrahedra. The C d06 octahedra with C d -0 distances between 2.24 and 2.31 A are strongly angle-distorted. Besides hydrogen bonds of medium strength (d0...o = 2.66 A) there are also much more weaker ones (d0...0 = 3.04 A). Considering these latter ones zigzag chains in z-direction can be recognized. The relatively low stability of Cd(H S04)2 in comparison with other metal-II-hydrogen sulfates is discussed with respect to its structural pecularities. 
  Reference    (Z. Naturforsch. 51b, 14—18 [1996]; eingegangen am 13. Juni 1995) 
  Published    1996 
  Keywords    Synthesis, Crystal Structure Zinc, Cadmium, Hydrogen Sulfate 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0014.pdf 
 Identifier    ZNB-1996-51b-0014 
 Volume    51 
169Author    S. Trojanov, A. Stiewe, E. KemnitzRequires cookie*
 Title    Synthese und Struktur saurer Ubergangsmetallsulfate - Ti(H50 2)(S 0 4)2(H20 ) 2 und Zr(H30 ) 2(S 0 4)3 Synthesis and Structure of Acid Transition Metal Sulfates - Ti(H50 2)(S 0 4)2(H20 )2 and Zr(H30 ) 2(S 0 4)3  
 Abstract    From the ternary system Mn(S 0 4)n/2 / S 0 3 / H20 (Mn+ = Zr4+, Ti3+) two new acid metal sulfates, Ti(H50 2)(S 0 4)2(H20)2 and Zr(H30) 2(S 0 4)3, have been synthesized and structurally characterized. Ti(H50 2)(S 0 4)2(H->0)i crystallizes in the orthorhombic space group Pnma with cell parameters a = 9.858(5), b = 18.32(2), c = 5.437(7)Ä (Z = 4); Zr(H30) 2(S 0 4)3 crystallizes in the triclinic space group PI with cell parameters a = 5.092(2), b = 8.533(3), c = 12.388(6)A, a = 92.95(3)°, ß = 90.89(3)°, 7 = 94.35(3)° (Z= 2). In the titanium compound there are slightly distorted T i0 6 octahedra with T i-0 distances between 1.99 and 2.09 A which are sharing corners with S 0 4 tetrahedra. Through hydrogen bonds layers are formed perpendicular to the 6-axis. These layers are connected by H30 + ions only. The structure of Zr(H30) 2(S 0 4)3 consists of three different S 0 4 tetrahedra and distorted Zr07 polyhedra which are connected via common corners and edges to form columns parallel to the a-axis. The Z r-0 distances vary from 2.13o to 2.18A for equatorial positions, significantly longer than the axial Zr-O distances with 2.05A. 
  Reference    (Z. Naturforsch. 51b, 19—24 [1996]; eingegangen am 13. Juni 1995) 
  Published    1996 
  Keywords    Synthesis, Crystal Structure, Titanium, Zirconium, Hydrogen Sulfates 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0019.pdf 
 Identifier    ZNB-1996-51b-0019 
 Volume    51 
170Author    Stefan Horstmann, Wolfgang SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumchlorid [P(NH2)4]C1 Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Chloride [P(NH2)4]C1  
 Abstract    [P(NH2)4]C1 has been prepared by ammonolysis of phosphorus pentachloride in liquid ammonia. The product was purified by reacting the byproduct, ammonium chloride, with diethylamine and removing the diethylamine hydrochloride. Suitable single crystals were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. The crystal structure of [P(NH2)4]C1 has been determined by single crystal X-ray methods (Pbcn, a = 470.8(2), b = 1622.3(3), c = 756.3(2) pm, Z = 4). In the solid, [PfNH2)4]+ and Cl~ ions are found, resembling a Til-analogous structure. The N -H -C l distances indicate N -H — Cl hydrogen bonding interactions. The distortion of the P-N sceleton of the cation and the very short P -N H 2 distances (mean value: 161.2 pm) have been confirmed by ab initio calculations, which show a generalized anomeric effect of the electron pairs at nitrogen and pjrdjr bonding. 
  Reference    (Z. Naturforsch. 51b, 127—132 [1996]; eingegangen am 18. Mai 1995) 
  Published    1996 
  Keywords    Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Vibrational Spectroscopic Data 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0127.pdf 
 Identifier    ZNB-1996-51b-0127 
 Volume    51 
171Author    Jochen Ellermann, Peter Gabold, FalkA. Knoch, MatthiasM. Oll, Astrid Schmidt, Martin SchützRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 120 [1] Synthesen und Kristallstrukturanalysen von Tris(imido-tetraphenyl- diphosphinato-0,0')eisen(III) und des PP-verknüpften Phosphazens Ph2P-N=PPh2-PPh2=N-PPh2 Chemistry o f Polyfunctional M olecules, 120 [11 Syntheses and Crystal Structures o f Tris(imido-tetraphenyl-diphosphinato-0,0')iron(III) and o f the PP-Connected Phosphazene Ph2P-N=PPh2-PPh2=N-PPh2  
 Abstract    While the reaction of anhydrous iron(III) chloride with the chelate ligand [(C6H5)2P(0)]2NH (6) is an efficient way to synthesize the new tricyclic compound imido-tetraphenyl-diphosphinato-0,0'iron(III), [Fe{0-P(Ph2)=N-P(Ph2)= 0 }3] (4), treatment of [(C6H5)2P]2NLi (1) with anhydrous iron(III) fluoride in THF represents a simple route to obtain the phosphorus-phosphorus connected species Ph2P-N=PPh2-PPh2=N-PPh2(7). Both compounds were charac­ terized by X-ray crystallography, 'H ,31 P {1H}, 13C {1H} NMR, IR, Raman and mass spectra. 
  Reference    Z. Naturforsch. 51b, 201—208 (1996); eingegangen am 24. Juli 1995 
  Published    1996 
  Keywords    Phosphazene, Iron Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0201.pdf 
 Identifier    ZNB-1996-51b-0201 
 Volume    51 
172Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0313.pdf 
 Identifier    ZNB-1996-51b-0313 
 Volume    51 
173Author    Karsten Bluhm, Andre WieschRequires cookie*
 Title    Synthese und Kristallstruktur von NiHo2(B20 5)2, das erste Nickellanthanoidborat mit einem ^ (B 20 5)4"-Anion Synthesis and Crystal Structure of NiHo2(B20 5)2, the First Nickel Lanthanoid Borates with a (^ (B 20 5)4" A nion  
 Abstract    Single crystals o f N iH o2(B20 5) 2 were prepared by a B20 3 flux-technique in high temperature reactions at 1450 °C and investigated by X-ray diffraction. They crystallize in the space group C 2h-P 2 ,/c (Nr. 14) with a = 451.0(4); b = 724.8(3); c = 938.8(6) pm; ß = 9 1 ,39(1)°; Z = 2. The compound is isotypic to CuTb2(B20 5) 2 as well as to the gadolinite structure (F eY 2 (B e S i0 5)2) and contains a two dimensional infinite anion with the formula 2 (B 2 0 5)4~. The borate layers consist o f four-and eight-membered rings o f edge-sharing B 0 4 tetrahedra. The layers are connected via copper-centered elongated oxygen-octahedra and slightly distorted tetragonal H o 0 8 antiprisms. 
  Reference    Z. Naturforsch. 51b, 677 (1996); eingegangen am 9. November 1995 
  Published    1996 
  Keywords    N ickel, Holmium, Borate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0677 
 Volume    51 
174Author    Cheong-HwaKarsten Park, BluhmRequires cookie*
 Title    Zur Synthese und Kristallstruktur von Bariumboroarsenat Ba(BAs05) mit einem Beitrag über Bariumorthoarsenat Ba3(As04)2 Synthesis and Crystal Structure of Barium Boroarsenate B a(B A s05) with a Contribution on Barium Orthoarsenate Ba3(A s0 4)2  
 Abstract    Single crystals of Ba(BAs05) (I) and Ba3(As04)2 (II) were obtained by melting B20 3, arsenic pentoxide and BaO at 1100°C. Both compounds crystallize trigonally, space groups (I): C3 -P3t (Nr. 144), (II): D3d -R3m (Nr. 166), with the lattice parameters (I): a = 726.7(1), c = 710.6(1) pm, Z = 3 and (II): a = 576.7(1), c = 2116.3(2) pm, Z = 3. Ba(BAsOj) is isotypic to Pb(BAs05) (Stillwellite structure) and Ba3(As04)2 to Ba3(P04)2. The structure of Ba(BAs05) is characterized by helical chains of rings of two borate tetrahedra and one arsenate tetrahedron. Barium is tenfold coordinated by oxygen. A rod-like sequence of coordination polyhedra, A s04-Ba(2)O|0-Ba(1)O|2-Ba(2)O|0-AsO4 is characteristic in the crystal structure of Ba3(A s04)2. 
  Reference    Z. Naturforsch. 51b, 722—726 (1996); eingegangen am 9. November 1995 
  Published    1996 
  Keywords    Barium Arsenic, Borate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0722 
 Volume    51 
175Author    C. W. Erner1, E. K. Em Nitza, H. W. Orzalab, S. TrojanovaRequires cookie*
 Title    Synthese und Kristallstruktur von Ba(H S04)2(H2S 0 4)3 und Sr(H S04)2(H2S 0 4) Synthesis and Structure o f B a (H S 0 4)2(H 2S 0 4)3 and S r(H S 0 4)2(H 2S 0 4)  
 Abstract    From the binary systems M 2S 0 4/H 2S 0 4 (M = Ba. Sr), two new hydrogen sulfates, (Ba(HS0 4)2(H 2S0 4)3 and S r(H S 04)2(H 2S 0 4), have been synthesized and structurally char­ acterized. Ba(HS0 4)2(H2S0 4)3 crystallizes in the orthorhombic space group P 2 12 12 , with unit cell parameters a = 4.680(1), b = 11.267(2), c = 29.188(6)A, Z = 4. B a 0 9 trigonal prismatic polyhedra with Ba-O distances of 2.68 -3.02 A from nine different S 0 4 tetrahedra are connected via common bases and build "isolated" columns consisting of O-S-O bridged double chains along the .r-axis. H S 0 4 and H2S 0 4 tetrahedra are linked via hydrogen bonds to form columns. S r(H S 04)i(H TS04) crystallizes in the triclinic space group P i with unit cell parameters a = 5.971(1), b = 8.468(2), c = 10.226(2)A, a = 81.71(3), ß = 83.30(3), 7 = 70.69(3)°, Z = 2. Sr is coordinated by nine oxygen atoms from seven different S 0 4 tetrahedra with S r-0 distances of 2.47 -2.84 A. The S r0 9 polyhedra build layers consisting of O-S-O bridged chains. Three crystallographically different S 0 4 tetrahedra are linked via hydrogen bonds to form a kind of flattened cylinder along the .v-axis. 
  Reference    Z. Naturforsch. 51b, 952—958 (1996); eingegangen am 15. Januar 1996 
  Published    1996 
  Keywords    Barium Hydrogen Sulfate Strontium Hydrogen Sulfate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0952 
 Volume    51 
176Author    J. BeckRequires cookie*
 Title    [TeCl3]+)3[MoCI6]2-(C  
 Abstract    The Reaction o f M oC 14 w ith TeCl4: Synthesis and Crystal Structure of Tris(trichlorotelluronium) H exachlorom olybdate(IV) Chloride, ([TeCl3]+)3[M oCl6]2-[ C l -] Red crystals of (T e C l^ M o C l^ C l) are obtained by reacting MoCl4 with TeCl4 in a 1:3 molar ratio in a sealed evacuated ampoule at 170°. The crystal structure determination (orthorhombic, space group Cmc2), a = 1541.6(2), b = 1268.1(1), c = 1180.6(1) pm) shows the presence of trigonal-pyramidal [TeCl3]+ ions, octahedral [MoCI(l]2-ions, and isolated C l-ions. The ions are linked by long Te-Cl bridges resulting in distorted TeCl(l octahedra. The octahedra are connected by joint edges and corners to zig-zag chains running along the polar c axis. 
  Reference    Z. Naturforsch. 51b, 1127—1131 (1996); eingegangen am 28. Februar 1996 
  Published    1996 
  Keywords    Trichlorotelluronium, Hexachloromolybdate(IV), Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1127 
 Volume    51 
177Author    Mitra Ghassemzadeh, Klaus Harms, Kurt DehnickeRequires cookie*
 Title    N ,N  
 Abstract    D im ethylharnstoff als chelatisierende Lewis-Säure: Synthese und K ristallstrukturen von PPh4[C l(H 2M e2N2CO)] und (PPh4)2[C l(H 2 M e2N2CO)]Cl N.N'-Dimethylurea as a Chelating Lewis Acid: Synthesis and Crystal Structures of PPh4[Cl(H2Me2N2CO)] and (PPh4)2[Cl(H2Me2N2CO)]Cl The title compounds have been prepared from tetraphenylphosphonium chloride and N,N'-dimethylurea in acetonitrile using different molar ratios of the educts. Both compounds were characterized by IR spectroscopy and by crystal structure determinations. PPh4[C l(H ,M e,N ,C O)l: Space group P i, Z = 4 ,a = 1021.8(2), b = 1192.7(2), c = 2143.9(4) pm, o = 87.21(3)°, ß = 85.95(3)°, = 74.16(3)° (-50°C). (PPh4MCl(H,Me-,N-,CO)]Cl: Space group P2,/n, Z = 4, a = 1138.4(2), b = 2855.4(3), c = 1394.0(1) pm, ß = 91.19(10)° (-60°C). In both compounds the N.N'-dimethylurea molecule acts as a chelating Lewis acid via two Cl -H hydrogen bonds forming nearly planar ClH 2N: C-six-membered heterocycles. 
  Reference    Z. Naturforsch. 51b, 1423—1427 (1996); eingegangen am 5. Juni 1996 
  Published    1996 
  Keywords    Chloride Complexes, NN'-Dimethylurea, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1423 
 Volume    51 
178Author    M. Itra, G. Hassem Zadeha, JörgM. Agullb, D. Ieter Fenskeb, KurtD. EhnickeaRequires cookie*
 Title    PPh4[Cl-I-C6H5] und PPh4[Br-I-C6H5] Iodobenzene as Lewis-Acid: Synthesis and Crystal Structures of PPh4[Cl-I-C6H5] and PPh4[Br-I-C6H 5]  
 Abstract    The donor-acceptor complexes [X-I-C6H5]~ with X" = Cl-and Br-have been prepared as tetraphenylphosphonium salts from iodobenzene and PPh4X in acetonitrile solutions. They form colourless single crystals, which were characterized by crystal structure determinations. PPh4[Cl-I-C6H5]: Space group P2,/c, Z = 4. Lattice dimensions at -70°C: a = 1301.1(5), 
  Reference    Z. Naturforsch. 51b, 1579—1582 (1996); eingegangen am 18. Juni 1996 
  Published    1996 
  Keywords    Halide Complexes of Iodobenzene, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1579 
 Volume    51 
179Author    M. M. Om, K. D. Ertza, Ehnickea ', J. M. AgullbRequires cookie*
 Title     
 Abstract    Colourless single crystals of the title compound are obtained from a saturated solution of NaOSiPh, in toluene in a humid atmosphere. We have characterized [N a ^ O S iP h ^ H iO),] by IR spectroscopy and by a crystal structure determination. Space group R3, Z = 6 , R -0.056. Lattice dimensions at -70°C: a -b = 1540.3 pm, c = 2639.6 pm. The compound has the structure of a Na40 4 heterocubane which is only slighty distorted and in which one of the sodium atoms is not hydrated and shows coordination number three. Die Kristallstruktur von [Na4(0SiPh3)4(H20)3] 
  Reference    Z. Naturforsch. 51b, 1583—1586 (1996); eingegangen am 9. Juli 1996 
  Published    1996 
  Keywords    Sodium Triphenylsilanolate Hydrate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1583 
 Volume    51 
180Author    P. Eter, G. JonesRequires cookie*
 Title     
 Abstract    o ly su lfo n y la m in e, L X X V III [1] l-M e sy l-4 -d im e th y la m in o p y r id in iu m -d im esylam id : D a r ste llu n g und F estkörperstru ktur Polysulfonylam ines, L X X V III [1] l-M esyl-4-dim ethylam inopyridinium D im esylam ide: Synthesis and Solid State Structure A n d reas W irth, A rm an d B laschette Treating (MeSC^X^N with 4-dimethylaminopy-ridine in MeCN afforded the ionic title compound (monoclinic, space group P2j/c). The bond lengths of the 4-dimethylaminopyridinium moiety suggest a semiquinoid resonance form with a dou­ ble bond to the exocyclic nitrogen and two local­ ized carbon-carbon double bonds in the ring. The ring and the exocyclic N and S atoms of the cation are essentially coplanar. The S -N bond distances in the cation (173.4 pm) and the anion (159.1 and 159.6 pm) correlate with Pauling bond orders of 1.0 and 1.7, respectively. The anion displays a staggered conformation with approximate C2 symmetry (S -N -S 120.4°). 
  Reference    Z. Naturforsch. 51b, 1666—1668 (1996); eingegangen am 20. August 1996 
  Published    1996 
  Keywords    l-Mesyl-4-dimethylaminopyridinium Dimesylamide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1666_n 
 Volume    51 
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