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Facet   Publication Year 1996  [X]
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1996[X]
1Author    Z. NaturforschRequires cookie*
 Title    A -P r 2S3, D -H o2S3 und E -Y b 2S3: Synthese und Einkristallstrukturuntersuchungen  
 Abstract    The oxidation of reduced chlorides (MC12) or chloride-hydrides (MC1HV) of the lanthani­ des with sulfur (700-850 °C, 7 d, sealed tantalum capsules or evacuated silica vessels) usually results in the formation of the sesquisulfides M2S3 as the main products. In the presence of appropriate fluxes (e.g., alkali halides), the products often are obtained as single crystals, and the flux decides which modification is favoured. Ternary halides of the trivalent lanthanides with the corresponding alkali metal can mostly be found as the second components. Crystal growth and structural investigations of thus produced single crystals of Pr2S3 (from PrClH() 67 + S + NaCl, 5:5:1, A type: orthorhombic, Pnma (No. 62), Z = 4, a = 748.22(5), b = 405.51(3), c = 1560.74(9) pm, R = 0.024, Rw = 0.020), Ho^S, (from U -H o^S , + KI, 1:1, D type: mono­ clinic, P 2xim (No. 12), Z = 6, a = 1746.15(9), b = 400.23(3), c = 1012.43(6) pm, ß = 98.529(4)°, R = 0.041, Rw = 0.035), and YbiS3 (from T-Yb^S^ + KI, 1:1, E type: trigonal, R 3c (No. 167), Z = 6, a = 674.97(2), c = 1820.11(9) pm'. R = 0.019, Rw = 0.018) are reported here. In accordance with the lanthanide contraction, the trivalent cations (M3+) exhibit sulfur coordination numbers of 7 and 8 in A -P r 2S3, 6 and 7 in D -H o 2S3, and 6 in E -Y b 2S3 (corundum-type structure). 
  Reference    Z. Naturforsch. 51b, 733—738 (1996); eingegangen am 4. Oktober 1994 
  Published    1996 
  Keywords    Lanthanides, Sesquisulfides, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0733.pdf 
 Identifier    ZNB-1996-51b-0733 
 Volume    51 
2Author    H. V., A. Fischerb, P. G. JonesbRequires cookie*
 Title    Eine unerwartete Synthese des Triphenyphosphazenium-chlorids, [(C6H5)3PNH2]+CI_ und eine Neubestimmung seiner Kristallstruktur  
 Abstract    Triphenylphosphazenium chloride has been prepared by the reaction of triphenylphos-phine with trimethylsilylazide in impure, wet dichloromethane. Yields are improved as stoi­ chiometric quantities of w ater are added. Colourless crystals are obtained by recrystallization from the same solvent. The crystals are triclinic, space group P I, Z=2, a = 894,6(3), b -979,8(3), c = 1142,9(4) pm, a = 107,27(3), ß = 93,70(3), y = 92,97(3)°. In the solid state the compound exists as [(C6H 5)3PNH2]+ cations, and Cl-anions. Dimeric units are formed by H-bonding. The crystal structure contains one molecule CH 2C12 per one molecule (C6H 5)3PNH2C1. The cation has a slightly irregular tetrahedral geometry around the P-atom with a relatively short P-N bond. 
  Reference    Z. Naturforsch. 51b, 865—868 (1996); eingegangen am 21. O ktober 1995 
  Published    1996 
  Keywords    Triphenylphosphazenium Chloride, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0865.pdf 
 Identifier    ZNB-1996-51b-0865 
 Volume    51 
3Author    G. Eorge Sosnovsky, Jan Lukszo, C. Ert, BraschRequires cookie*
 Title    Preparation of an Aminoxyl Analog of the Anticancer Agent Miltefosine  
 Abstract    The synthesis and a few properties of hexadecyl 2-[N,N-dimethyl-N-(2,2,6.6-tetramethyl-l-oxyl-piperidin-4-yl)ammonio] ethyl phosphate are described. This compound is a spin la­ beled analog of the antineoplastic drug hexadecylphosphocholine (Miltefosine). 
  Reference    Z. Naturforsch. 51b, 888—890 (1996); received Decem ber 11 1995 
  Published    1996 
  Keywords    Anticancer Agents, Aminoxyl, Nitroxyl, Synthesis 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0888.pdf 
 Identifier    ZNB-1996-51b-0888 
 Volume    51 
4Author    N. Stock, W. SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von l,l>3 ?3 ?3 -Pentaam*n° -l  
 Abstract    oxo-lA 5 ,3A 5 -diphosphaz-2-en, (NH2)2 (0)P-N=P(NH2)3 Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam ino-l-oxo-l A 5 , 3 A 5 -diphosphaz-2-ene, (NH2)2(0)P-N =P(N H i)3 Coarse crystalline (NH2)2(0)P-N=P(NH2)3 is obtained from a NH;* saturated CH2C12 suspen­ sion of (NH2)2(0)P-N=P(NH2)3 NH4C1 at room temperature. (NH2)2(0)P-N=P(NH2)3 NH4C1 is synthesized" by slow addition of C12(0)P-N=PC13 to a solution of NH3 in CH2C12 at -78 °C. Excess NH4C1 is removed by treatment with HNEt2 followed by extraction with CH2C12. The crystal structure of (NH2)2(0)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P2(/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, /3 = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H- • N > 313 pm. N-H • 0 > 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C. 
  Reference    Z. Naturforsch. 51b, 1079—1083 (1996); eingegangen am 7. Dezember 1995 
  Published    1996 
  Keywords    Aminophosphazene, Synthesis, Crystal Structure Precursor 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1079.pdf 
 Identifier    ZNB-1996-51b-1079 
 Volume    51 
5Author    Wolfgang Czado, Ulrich MüllerRequires cookie*
 Title    (PPh4)4Sb8Br28 Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28  
 Abstract    The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloro-methane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, a = 102.93(2), ß = 100.83(2), 7 = 100.42(2)°, Z = 2, triclinic, space group P I . (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284~ ion can be taken as the association product of eight SbBr3 molecules with four B r-ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres. Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), 
  Reference    Z. Naturforsch. 51b, 1245—1247 (1996); eingegangen am 22. März 1996 
  Published    1996 
  Keywords    Ocataikosabromooctaantimonate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1245.pdf 
 Identifier    ZNB-1996-51b-1245 
 Volume    51 
6Author    StefanH. Orstm, AnnW. Olfgang SchnickRequires cookie*
 Title    Synthese  
 Abstract    , K rista llstru k tu r und Eigenschaften von 1 ,1 , 1 > 3 * 3 , 3 -H e x a a m i n o -lA 5,3A5-diphosphazenium ehlorid[(N H 2)3PNP(NH2)3]Cl Synthesis, C rystal Structure, and Properties of 1,1,1,3,3,3-Hexaam ino-1 A5,3A5-diphosphazenium Chloride [(N H 2)3PN P(N H 2)3]C1 [(NH2)3PNP(NH2)3 ]C1 has been prepared by a three step synthesis. The last step is the ammo-nolysis of [C13PNPC13]C1. Single crystals of 1,1,1,3,3,3-hexaamino-1 A \ 3As-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -1 0 0 °C [(NH2)3PNP(NH2)3]C1 is sub­ ject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P i, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, ß = 76.36(3)°, 7 = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles. 
  Reference    Z. Naturforsch. 51b, 1732—1738 (1996); eingegangen am 26. Juni 1996 
  Published    1996 
  Keywords    Aminophosphazenes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1732.pdf 
 Identifier    ZNB-1996-51b-1732 
 Volume    51 
7Author    G. Rebe, Frank Weller, Kurt Dehnicke, ProfRequires cookie*
 Title    Jutta  
 Abstract    N-Iodo-triphenylphosphaneimine, Ph3PNI, has been prepared by thermolysis of the donor acceptor complex [Me3SiNPPh3-ICl] in boiling acetonitrile in the presence of potassium fluo­ ride. Both compounds have been characterized by IR spectroscopy and by crystal structure determinations. [Me3SiNPPh3 ICl]: Space group P I, Z = 2, a = 888.3(1), b = 1070.7(1), c = 1310.2(1) pm, a = 9 5 .15(1)°, ß = 108.67(1)°, 7 = 97.78(1)° at 20°C. The complex has a molecular structure in which the N atom of the phosphaneimine is connected with the iodine atom of the IC1 molecule in a linear arrangement N-I-Cl with bond lengths N-I = 232.7 pm, I-Cl = 255.37 pm. Ph3PNI: Space group P2,/n, Z = 4, a = 952.8(1), b = 1800.8(2), c = 1003.6(1) pm, ß = 110.25(1)° at -50°C. The compound forms monomeric molecules with bond lengths PN = 159.1 pm, I-N = 205.6 pm and an INP bond angle of 113.3°. N-Iod-triphenylphosphanimin. Synthese und Kristallstrukturen von [Me3SiNPPh3 ICl] und Ph3PNI 
  Reference    Z. Naturforsch. 51b, 1739—1743 (1996); eingegangen am 12. April 1996 
  Published    1996 
  Keywords    Phosphaneimine Complexes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-1739.pdf 
 Identifier    ZNB-1996-51b-1739 
 Volume    51 
8Author    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 
9Author    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 
10Author    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 
11Author    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 
12Author    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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 Identifier    ZNB-1996-51b-0201 
 Volume    51 
13Author    Park, K. Arsten BluhmRequires cookie*
 Title    Pb6(A s0 4)  
 Abstract    [B (A s04)4] -ein neuartiger Kristallstrukturtyp im System Pb0 /B2 0 3 /As2 0 5 mit einem Beitrag über P b(B A s05) Pb6(A s 0 4)[B (A s 0 4)4] -a New Crystal Structure Type in the System P b 0 /B 20 3/A s20 3 w ith R em arks about P b (B A s0 5) C heong- Single crystals of Pb6(A s04)[B(As04)4] (I) and Pb(BAs05) (II) were obtained by melting B->03, As20 5 and PbO at 800 °C. X-ray investigation led to the space group (I): S4 -P4 (Nr. 81) with a = 715.4(1), c = 976.2(3) pm, Z = 1 and (II): C | -P3, (Nr. 144) with a = 712.2(1), c = 693.5(2) pm, Z = 3. While (II) is isotypic to the Stillwellite structure, Pb^(As04)[B(As04)4] represents a completely novel type of crystal structure. Boron and arsenic are tetrahedrally coordinated by oxygen. These polyhedra form two kinds of isolated anions: A s04'~ and B(A s04)49_. Lead is eightfold coordinated by oxygen. 
  Reference    Z. Naturforsch. 51b, 313—318 (1996); eingegangen am 16. Oktober 1995 
  Published    1996 
  Keywords    Lead, Arsenic, Borate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0313 
 Volume    51 
14Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0677.pdf 
 Identifier    ZNB-1996-51b-0677 
 Volume    51 
15Author    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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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0722.pdf 
 Identifier    ZNB-1996-51b-0722 
 Volume    51 
16Author    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 
17Author    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 
18Author    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 
19Author    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 
20Author    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 
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