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'Synthesis' in keywords Facet   section ZfN Section B:Volume 053  [X]
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1998 (12)
1Author    G. Waidmann, M. JansenRequires cookie*
 Title    Synthese und Charakterisierung des Fulleren-Kokristallisats C60*SiH(C6H5)3 Synthesis and Characterisation of the Fullerene Co-Crystal C60*SiH(C6H5)3  
 Abstract    A new fullerene co-crystal C60*SiH(C6H5)3 has been synthesized by crystallisation from a melt of SiH(C6H5)3 and C60 in sealed duran tubes at 80°C. X-ray investigations led to triclinic symmetry, space group P i, a = 10.086(1),/? = 14.431(2), c = 14.911(2) Ä, a = 79.13(1), ß = 74.943(9), 7 = 88.33(1)°, V = 2058.0(4) A 3, Z = 2. The crystal structure consists of isolated fullerene and silane molecules. At -80°C, C60 is still rotationally disordered. Temperature dependent Guinier powder diagrams do not show any phase transformation between 25 and -165°C. The compound is stable in air. 
  Reference    Z. Naturforsch. 53b, 161—164 (1998); eingegangen am 14. November 1997 
  Published    1998 
  Keywords    Fullerene C60, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0161.pdf 
 Identifier    ZNB-1998-53b-0161 
 Volume    53 
2Author    Thorsten Grob, FrankW. Eller, K. Urt, D. EhnickeRequires cookie*
 Title    Die Kristallstruktur von [Me3PN(H)PMe3]4l 28? einem Polyiodid mit I3~-, lg2--und I144"-Ionen Crystal Structure o f [M e3P N (H )P M e3]4I28, a Polyiodide w ith I3~, I82 -, and I 144~ Ions  
 Abstract    Black-red single crystals of [Me3PN(H)PMe3]4I28 have been prepared by the reaction of [Me3PNPMe3]I with iodine in dichloromethane solution in the presence of Me3SiI and traces of water. The polyiodide crystallizes triclinically in the space group Pi with two formula units per unit cell with the lattice dimensions a = 831.2(1), b = 1661.2(3), c = 1739.0(3) pm, q = 87.26(1)°, ß = 79.48(1)°, 7 = 78.17(1)°. The structure consists of [Me3PN(H)PMe3]2+ ions, linear I3~ ions, z-shaped I8: ~ ions, and zig-zag chains of I I44-ions, the terminal iodine atoms of which form I-H -N hydrogen bridges to the cations. 
  Reference    Z. Naturforsch. 53b, 552—556 (1998); eingegangen am 23. Februar 1998 
  Published    1998 
  Keywords    Polyiodide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0552.pdf 
 Identifier    ZNB-1998-53b-0552 
 Volume    53 
3Author    Wieslawa KudelskaRequires cookie*
 Title    Synthesis of Glycosyl Cyanides by the Reaction of 1-5-Phosphorothioates of Carbohydrates with Trimethylsilyl Cyanide  
 Abstract    A new procedure is described for the synthesis of a,/?-glycosyl cyanides by the reaction of per-O-benzylated S-a-D-glycopyranosyl phosphorothioates with trimethylsilyl cyanide in the presence of Lewis acid. Starting S-glycosyl phosphorothioates are prepared, directly, from O-benzyl protected reducing D-hexopyranoses (gluco-, galacto-, manno-) and alkylammonium salt of phosphorothioic acid under Lewis acid catalysis. 
  Reference    Z. Naturforsch. 53b, 1277—1280 (1998); received July 23 1998 
  Published    1998 
  Keywords    S-Glycosylphosphorothioates, Glycosyl Cyanides, Synthesis 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1277.pdf 
 Identifier    ZNB-1998-53b-1277 
 Volume    53 
4Author    Andre Wiesch3, Hauke Timmb, Karsten Bluhm3Requires cookie*
 Title    Uber CuDy2[B80 16] und CuHo2[B80 16]: Zwei neue "Metaborate" mit einem ^ [B80 16]g_-Anion On CuDy2[B80 16] and CuHo2[B80 16]: Two New "Metaborates" with a ^ [B80 16]8-Anion  
 Abstract    Nearly colourless single crystals of the compounds CuDy2 [B80 i 6] (I) and CuHo2[B80)6] (II) have been obtained by a B20 3 flux technique. They crystallize in the structure of CuTb2 [B80)6] (I) or in an orthorhombic variant (II). X-ray investigations on single crystals led to the space group C2h -P2!/c (Nr. 14) with lattice parameters a = 1025,5(10); b = 836,99(10); c = 621,2(8) pm, ß = 90.47(10)°; Z = 2 (I) and D^h -Pbam (Nr. 55) with a = 840,7(2), b = 616,6(2), c = 1022,0(2) pm, Z = 2 (II). The structures contain 1 [B80 16]8_ chains isolated from each other, which include tri-and tetracoordinated boron, T'fie chains consist of alternating twelve and eight-membered rings of boron and oxygen atoms connected by B 0 4 units. Dy,+ and H o 3+ are octacoordinated and Cu2+ is hexacoordinated in elongated octahedra by oxygen. The relation between these two structures is discussed. 
  Reference    (Z. Naturforsch. 53b, 1—4 [1998]; eingegangen am 23. Oktober 1997) 
  Published    1998 
  Keywords    Copper, Lanthanoids, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0001.pdf 
 Identifier    ZNB-1998-53b-0001 
 Volume    53 
5Author    Lanthanoid Borates, A. Wiesch, K. BluhmRequires cookie*
 Title    CuHo2[B20 5]2* Ein unerwarteter Strukturtyp in der Reihe der Kupferlanthanoidborate CuHo2[B20 5]2: An Unexpected Structure Type in the Series of Copper  
 Abstract    Single crystals of the new compound CuHo2 [B20 5 ]2 were obtained by using a B20 3 flux technique with CuO and Ho20 3 at 1050 °C. X-ray investigations on single crystals led to the space group P 2,/c (Nr. 14) with lattice parameters a = 454.3(2); b = 726.0(4); c = 936.0(5) pm; ß = 90.77(1)°; Z = 2. The compound is isotypic to CuTb2[B20 5 ] 2 as well as to the gadolinite structure (FeY2 [BeSi05]2). The structure exhibits layer-like 2 [B20 5]4~, a two-dimensional anion consisting of edge sharing B 0 4 -tetrahedra, which form four-and eight-membered rings. The layers are connected by elongated C u06-octahedra and slightly distorted tetragonal LnOs-antiprisms. 
  Reference    (Z. Naturforsch. 53b, 5—8 [1998]; eingegangen am 23. Oktober 1997) 
  Published    1998 
  Keywords    Copper, Holmium, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0005.pdf 
 Identifier    ZNB-1998-53b-0005 
 Volume    53 
6Author    Helical Borate, AnionA. Wiesch, K. BluhmRequires cookie*
 Title    Ag2Cs[B1 5 0 2 4]* Ein wasserfreies quaternäres SiIber(I)-Borat mit einem neuartigen Boratanion mit helixartigem Aufbau Ag2C s[B 150 24]: An Anhydrous Quaternary Silver(I)-Borate with a New  
 Abstract    Single crystals o f Ag2C s[B ,50 24] were prepared by using a B 20 3 flux technique with Ag2C 0 3 and Cs2C 0 3 in a closed silver tube at 650 °C. X-Ray investigations led to a new crystal structure in the space group P 2 ,2 ,2 (Nr. 18) with lattice parameters a = 1778.7 (4); b = 2219.2 (4); c = 512.2 (1) pm, Z = 4. The silver atoms are part of distorted A g 0 4 tetrahedra and planar A g 0 3 units while the caesium atoms are eightfold coordinated by oxygen. The compound contains an as yet unknown borate anion [B,50 24] with twelve B 0 3-and three B 0 4 units per formula. The B 0 3 units are connected to eight cords twisted to helices which are combined via B 0 4 tetrahedra to a three dimensional framework with large tunnels occupied by the cations. 
  Reference    Z. Naturforsch. 53b, 157—160 (1998); eingegangen am 23. Oktober 1997 
  Published    1998 
  Keywords    Silver, Caesium, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0157.pdf 
 Identifier    ZNB-1998-53b-0157 
 Volume    53 
7Author    Hans-Friedrich Klein, Alexandra Brand, Gerhard CordierRequires cookie*
 Title    Synthesis and Reactions with CO and C2H4 of Cobalt(I) Complexes Containing Trimethylphosphine and Chelating o-Diphenylphosphanyl- phenolate Ligands  
 Abstract    In tetracoordinate cobalt(I) halide compounds CoX(Ph2P ^ O H)(P M e3)2 (X = CI, Br) o-phos-phanylphenols PhaP^O H are coordinated as phosphane ligands. In the presence o f base chelat­ ing anions Ph2P ^ O _ give rise to pentacoordinate com plexes Co(Ph2 P ^ O)(P M e3)3. M olec­ ular structures are presented for both types o f compounds. The five-membered chelate ring in Co(Ph2P ^ O)(P M e3)3 is resistant to protonation, and ring-opening is not observed in the presence o f CO or C2H4. Replacing one o f the trimethylphosphanes by one o f the 7r-acceptor ligands affords fiuxional com plex m olecules which upon cooling attain definite ground-state geometries out o f a multitude o f possible isomers. 
  Reference    Z. Naturforsch. 53b, 307 (1998); received November 28 1997 
  Published    1998 
  Keywords    Cobalt, o-Phosphanylphenolate Complexes, Synthesis, Structure, Fluxionality 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0307.pdf 
 Identifier    ZNB-1998-53b-0307 
 Volume    53 
8Author    LacknerRequires cookie*
 Title    Octacidomycine, IV : Neue Totalsynthese von rac-Octacidomycin und strukturverwandten Oligocarbonsäuren Octacidom ycins, I V : A New Total Synthesis of rac-O ctacidom ycin and Structurally R elated O ligocarboxylic A cids A ndreas K rause, H elm ut  
 Abstract    a new strategy, an improved total synthesis of the unique antibiotic octacidomy-cin (1) and of structurally related oligocarboxylic acids was developed (Scheme 1,2). Starting from 3 and the tetraethylester of l,17-dibromo-6,6,12,12-heptadecane-tetracarboxylic acid (6) as a key compound, systematical fragment condensations lead to the nonatriacontane-pentadecacarboxylic acid 11 and hence to the 1,3,9,15,21,27,33,39-nonatriacontane-octacarbo-xylic acid 1. The synthetic pathway can easily be modified and generally be applied for the synthesis of a broad variety of hitherto unknown oligocarboxylic acids or their esters, respec­ tively, and even of cyclic analogues (Scheme 2). 
  Reference    Z. Naturforsch. 53b, 1043—1050 (1998); eingegangen am 22. Juni 1998 
  Published    1998 
  Keywords    Antibiotics, Octacidomycins, Oligocarboxylic Acids, Synthesis, NMR Data Following 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1043.pdf 
 Identifier    ZNB-1998-53b-1043 
 Volume    53 
9Author    U. Steiner, W. ReicheltRequires cookie*
 Title    Zum System Sr/Mo/O: Phasendiagramm, Synthese und Charakterisierung der ternären Verbindungen On the System Sr/Mo/O: Phase Diagram, Synthesis and Characterization of Ternary Compounds  
 Abstract    The phase diagram of the ternary system Sr/Mo/O has been determined at a temperature of 1000°C. Powder samples of the ternary compounds SrM o04, Sr3M o06, SrM o03, Sr2M o04 and SrMo50 8 were prepared by solid state reactions. The thermochemical data of all ternary compounds were determined.oA new compound, Sr3Mo20 7, with a layered perovskite structure (a = 3.967(1), c = 20.588(5) A, I4/mmm) was found. Rietveld analysis based on powder X-ray diffraction data confirms that the compound Sr2M o04 has the K7NiF4 structure (I4/mmm) with a = 3.9176(1), c = 12.8545(4) A. 
  Reference    (Z. Naturforsch. 53b, 110—116 [1998]; eingegangen am 10. Oktober 1997) 
  Published    1998 
  Keywords    Strontium Molybdate, Phase Diagram, Synthesis, Thermochemical Data, Electric Properties 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0110.pdf 
 Identifier    ZNB-1998-53b-0110 
 Volume    53 
10Author    Gabriele Korus, Martin JansenRequires cookie*
 Title    Kristallstruktur von Natriumtrifluormethylsulfonat- Trifluormethylsulfonsäure (1/3) Studies on Sodium Trifluoromethanesulfonate. Crystal Structure of Sodium Trifluoromethanesulfonate-Trifluoromethanesulfonic Acid (1/3)  
 Abstract    Single crystals of sodium trifluoromethanesulfonate-trifluoromethanesulfonic acid (1/3) (N aS 0 3CF3 • 3 H S 0 3CF3) have been prepared by reaction of sodium trifluoromethanesulfonate with anhydrous trifluoromethanesulfonic acid at 60 °C. N aS 0 3CF3 • 3 H S 0 3CF3 crystallizes in space group 1 2 ^ (No. 199) with a = 16.210(1) A, Z = 8. Sodium is coordinated by six oxygen atoms from six different trifluoromethanesulfonic acid molecules, each acid molecu­ le connecting two sodium ions. The 3-dimensional network resulting from the edge sharing octahedra corresponds to the cubic (10, 3) net, not realised otherwise, so far. The trifluorome­ thanesulfonate anion is bonded to three trifluoromethanesulfonic acid molecules by hydrogen bonds. 
  Reference    Z. Naturforsch. 53b, 438—442 (1998); eingegangen am 19. Dezember 1997 
  Published    1998 
  Keywords    Sodium Trifluoromethanesulfonate, Sodium Triflate, Trifluoromethanesulfonic Acid, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0438.pdf 
 Identifier    ZNB-1998-53b-0438 
 Volume    53 
11Author    ViktorP. Balema, Steffen Blaurock, Evamarie Hey-HawkinsRequires cookie*
 Title    Synthesis and Molecular Structure of a Superbulky Tertiary Phosphine: Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine  
 Abstract    Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine (2) was obtained in 91% yield from phenyldichlorophosphine and two equivalents of l-lithium-2-phenyl-l ,2-dicarba-c/o5o-dodecaborane(12) in ether and characterized by spectroscopy (3IP, 1 B, 'H, l3C NMR; IR) and by X-ray structure determination. 
  Reference    Z. Naturforsch. 53b, 1273—1276 (1998); received May 20 1998 
  Published    1998 
  Keywords    Synthesis, Molecular Structure, X-Ray Data, NMR Data, Phosphine 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1273.pdf 
 Identifier    ZNB-1998-53b-1273 
 Volume    53 
12Author    JonesRequires cookie*
 Title    Polysulfonylamine, CV [1] Die ersten N,N-disulfonylierten Sulfinsäureamide: Synthese und Kristallstrukturen von R S ( 0 )-N (S 0 2Me)2 (R = Me, CC13)  
 Abstract    P o ly su lfo n y lam in es, C V [1] T h e F irst N ,N -D isu lfo n y lated S ulfinic A m id es: S y nthesis a n d C ry sta l S tru c tu re s o f R S (0) -N (S 0 2M e)2 (R = M e, CC13) M a rtin a N äv e k e, A rm a n d B lasc h ette* , P e te r G. The novel sulfinamides R S (0) -N (S 0 2M e)2, where R = Me (la) or CC13 (lb), were ob­ tained by treating the corresponding sulfinyl chlorides with Me3S iN (S 02Me)2 or AgN-(S 0 2Me)2, respectively. A presumedly ionic 1:1 adduct of lb with 4-dimethylaminopyridine was isolated and analytically characterized. In the crystals of la (monoclinic, space group P2\!ri) and lb (monoclinic, P l j c) , the molecules feature approximately planar NS3 moieties, unusually long S (0) -N bonds and, in the case of lb, an extremely long S (0) -C bond [for la and lb, in order: sum of bond angles at nitrogen 359.5 and 357.1°, S (0) -N 178.2(2) and 173.6(2) pm, S (0) -C 178.8(2) and 194.1(2) pm]. In both molecular structures, an attractive S (0) --0 1,4-interaction leads to a 7.3° discrepancy in the S (0) -N -S 0 2 angles. The crystal packing of la displays a tape (double-chain) motif generated by two prominent intermolecu-lar C -H -O interactions involving one M e S 0 2 group and the sulfinyl oxygen atoms of two adjacent molecules, whereas in lb the molecules are associated into parallel chains via a bonding C l-"0(sulfonyl) interaction. 
  Reference    Z. Naturforsch. 53b, 734—741 (1998); eingegangen am 6. April 1998 
  Published    1998 
  Keywords    N, N-Bis(organosulfonyl)sulfinamides, Synthesis, Crystal Structure, Long S ( 0 ) -N Bond 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0734.pdf 
 Identifier    ZNB-1998-53b-0734 
 Volume    53