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1998[X]
21Author    Andreas Mommertz, Roland Leo, Werner Massa, Kurt DehnickeRequires cookie*
 Title    Uber die Reaktion von Bis(f-butylamino)dimethylsilan mit Titantetrachlorid. Kristallstrukturen des Imido-Komplexes [TiCl2 (N-CMe3 )(H2 N-CMe3 )(CH3CN)]2 und des Ketimido-Komplexes [TiCl3 {NC(Me)N(H)CMe3}(CH3CN)2 ]  
 Abstract    On the Reaction of Bis(f-butylamino)dimethylsilane with Titanium Tetrachloride. Crystal Structures of the Imido Complex [TiCl->(N-CMe3)(H-,N-CMe3)(CH3CN)]2 and of the Ketimido Complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] The reaction of bis(f-butylamino)dimethylsilane with titanium tetrachloride in dichloro­ methane solution leads to a mixture of compounds from which the imido complex (H3N-CMe3)2[TiCl3(N-CMe3)]2 (1) and by extraction of the residue with acetonitrile the imido complex [TiCl2(N-CMe3)(H2N-CMe3)(CH3CN)]2 (2) can be isolated. 1 reacts with acetonitrile to give the ketimido complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] (3). According to crystal structure determinations 2 consists of centrosymmetric dimeric molecules containing TiCl2Ti bridges, the N-CMe3~ ligands being in equatorial positions with TiN bond lengths of 168.8(4) pm which corresponds to double bonds. In the monomeric complex 3 the chloro ligands are in meridional positions of the distorted octahedrally coordinated titanium atom with a TiN bond length of 175.7(2) pm of the ketimido ligand. 
  Reference    Z. Naturforsch. 53b, 887—892 (1998); eingegangen am 27. April 1998 
  Published    1998 
  Keywords    Titanium, Imido Complex, Ketimido Complex, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0887.pdf 
 Identifier    ZNB-1998-53b-0887 
 Volume    53 
22Author    Werner Urland, Helmut PersonRequires cookie*
 Title    Zur Kristallstruktur von Ho2Se3 On the Crystal Structure of Ho2Se3  
 Abstract    Starting from HoSe2_ t powder and holmium metal bright brownish-yellow, plate-like single crystals of Ho2Se3 could be prepared by chemical transport with A1C13. Holmium sesquiselenide crystallizes in the Sc2S3-type structure, space group Fddd, with lattice constants a = 1140,7(2), b -812,6(1) and c = 2423,9(3) pm. 
  Reference    Z. Naturforsch. 53b, 900—902 (1998); eingegangen am 9. April 1998 
  Published    1998 
  Keywords    Holmium Sesquiselenide, Chemical Transport, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0900.pdf 
 Identifier    ZNB-1998-53b-0900 
 Volume    53 
23Author    Isabel Díaza, Vicente Fernández, José Luis, M. Artínezb, Lothar Beyer0, Astrid Pilzd, Ulrich MüllerdRequires cookie*
 Title    Thermochrome Chloro-und Bromocuprate  
 Abstract    [C(NH2)3]2[CuBr4], (H3CC2N2SNH3)2[Cu2Br6], (C7N3H14)2[CuC14], (C7N3H14)2[CuBr4], [(Cl, Br)C3N2H6][CuCl3OH2] und (BrC3N2H6)2[CuBr4] Thermochromic Chloro-and Bromocuprates: [C(NH2)3]2CuBr4, (H3CC2N9SNH3)2[Cu2Br6], (C7N 3H 14)2[CuC14], (C7N3H 14)2[CuBr4], [(Cl, Br)C3N2H6][CuCl3OH2] and (BrC3N2H6)2[CuBr4] CuCl2 and CuBr2 were reacted in water-ethanol solutions containing HC1 or HBr, re­ spectively, with the following organic bases or their chlorides or bromides: guanidine (1), 2-amino-5-methyl-l,3,4-thiadiazol (2), hexahydro-2//-pyrimidine-(1,2A)-pyrimidine (3), and 2-hydrazino-2-imidazoline (4). With 1 and 3 the tetrahalocuprates (lH)2[CuBr4], (3H)2[CuCl4] and (3H)2[CuBr4] were obtained having flattened tetrahedral anions. 2 and CuBr2 form (2H)2[Cu2Br6], with nearly planar [Cu2Br6]2-ions that are associated to chains with square-pyramidal coordination of Cu. 2 and CuCl2 yield the hydrate (2H)C1H20 . 4 undergoes substitution of the hydrazine group for halogen, yielding the 2-halo-2-imidazolinium salts (5H)0 2(6H)o,8[CuCl3OH2] and (6H)2[CuBr4] in addition to [H3NCH2CH2NH3][CuCl4] (5 = 2-chloro-, 6 = 2-bromo-2-imidazoline). The planar [CuCl3(OH2)]_ ions are associated to chains. Crystal structure determinations were performed with (lH)2[CuBr4], (2H)2[Cu2Br6], (3H)2[CuCl4], (5H)0 2(6H)o 8[CuCl3OH2] and (6H)2[CuBr4]; the latter three at 298 K and at 166 K or 173 K. The known crystal structure of [H3N(CH2)2NH3][CuCl4] was redetermined at 166 K. In all cases small differences of bond lengths and bond angles are observed between room temperature and low temperature. The magnetic properties and electrospray mass spectra were measured. The products show thermochromic behavior. 
  Reference    Z. Naturforsch. 53b, 933—938 (1998); eingegangen am 6. Mai 1998 
  Published    1998 
  Keywords    Chloro Cuprates, Bromo Cuprates, Crystal Structures, Thermochromism 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0933.pdf 
 Identifier    ZNB-1998-53b-0933 
 Volume    53 
24Author    Steffen Runge, M. Athias, O. SengeRequires cookie*
 Title    Electron Donor-Acceptor Compounds. Synthesis and Structure of 5-(l,4-Benzoquinone-2-yl)-10,15,20-trialkylporphyrins  
 Abstract    A series of 5-(benzoquinone)-10,15,20-trialkylporphyrins was synthesized via cross conden­ sation of the respective aldehydes, 2,5-dimethoxybenzaldehyde and pyrrole followed by de-methylation with BBr3 and oxidation with P b 0 2. This method worked reasonably well for compounds bearing the benzoquinone substituent and butyl, isopropyl, 1 -methylpropyl and 2-ethylpropyl residues (2a-d). The free base porphyrin quinones were converted into the zinc(II) complexes (3a-d) all of which showed remarkable stability for porphyrin quinones. The zinc(II) complex 3c bearing isopropyl residues was investigated by X-ray crystallography and showed a supramolecular structure consisting of polymeric chains facilitated by coordina­ tion of a benzoquinone oxygen to a neighboring zinc(II) center. Attempts to synthesize a 5-(benzoquinone)-10,15,20-tris(terr-butylporphyrin) resulted in the formation of a yellow por-phomethene (4), which could not be oxidized further. A crystal structure analysis of 4, the first for a free base porphomethene, shows an extremely twisted conformation with syn-orientation of the three rm-butyl groups. The results indicate that new methods will have to be developed for the synthesis of nonplanar porphyrin quinones. 
  Reference    Z. Naturforsch. 53b, 1021—1030 (1998); received June 15 1998 
  Published    1998 
  Keywords    Porphyrins, Quinones, Electron Transfer Compounds, Crystal Structure, Conformation 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1021.pdf 
 Identifier    ZNB-1998-53b-1021 
 Volume    53 
25Author    M. Sm, B. Ern, H. Ard, N. Eum Üller, K. Urt, D. EhnickeRequires cookie*
 Title    ClPb[N(SiMe3)2]3 C rystal S tructure of C lPb[N (SiM e3 ) 2 ]3  
 Abstract    Pale brown single crystals of the title compound have been obtained by the reaction of Pb[N(SiMe3) 2] 2 with molybdenum pentachloride in ether solution as a result of a redox reaction. ClPb[N(SiMe3) 2] 3 crystallizes in the trigonal space group R3 with three formula units per unit cell. Lattice dimensions at -50 °C: a = b -1828.7(2), c = 854.5(1) pm. The compound forms monomeric molecules with bond lengths P b-C l = 247.9(4) pm and P b -N = 213(2) pm. 
  Reference    Z. Naturforsch. 53b, 1074—1076 (1998); eingegangen am 3. Juli 1998 
  Published    1998 
  Keywords    Lead(IV), Amido Complex, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1074_n.pdf 
 Identifier    ZNB-1998-53b-1074_n 
 Volume    53 
26Author    Frank Wendland, Christian Näther, Michael Schur, Wolfgang BenschRequires cookie*
 Title    Solvothermal Synthesis and Crystal Structure Determination of Tris- (ethyleneamine-ammonium) Tetraselenoantimonat: Non-Centrosymmetry Mediated by an Extended Unusual N-H***N Hydrogen Bonded Network?  
 Abstract    The title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe,*3 --anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction. 
  Reference    Z. Naturforsch. 53b, 1144—1148 (1998); received June 15 1998 
  Published    1998 
  Keywords    Selenoantimonates, Solvothermal Synthesis, Crystal Structure, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1144.pdf 
 Identifier    ZNB-1998-53b-1144 
 Volume    53 
27Author    Markus Tampier, Dirk JohrendtRequires cookie*
 Title    B aC u 6G e2S8 -Ein Thiogermanat als Variante der L i3Bi-Struktur BaCu6Ge2S8 -A Thiogermanate as a Variant of the Li3Bi Structure  
 Abstract    BaCu6Ge2S8 was synthesized by direct reaction of the elements at 750°C and characteri­ zed by X-ray single crystal techniques. The thiogermanate crystallizes in a new orthorhombic structure type (a = 6.122(1) A, b = 12.084(3) A , c = 17.614(5) A; Pbcm, Z = 4). Isola­ ted [GeS4]4_ tetrahedra form a slightly distorted cubic face-centered (fee) arrangement. Ba-and Cu-atoms each occupy half the octahedral gaps (O G) of this " tetrahedra packing" . Fur­ ther Cu atoms fill the tetrahedral gaps (T G) completely. The compound can be written as Ba2<l/2 0 G,(Cu2)2<l/2<:)G)Cu8<7G)(GeS4)4 . Thus the structure o f BaCu6Ge2S8 can be derived from the Li^Bi type. The sulfur coordination o f the metal atoms (Cu tetrahedral or trigonal, Ba with CN 8) are realized by the spatial orientation of the [GeS4]4~ tetrahedra. Their centers nearly maintain the fcc-arrangement. This structure interpretation of BaCu6 Ge2S8 from the viewpoint o f a " filled tetrahedra packing" is discussed for further known thiogermanate compounds. 
  Reference    Z. Naturforsch. 53b, 1483—1488 (1998); eingegangen am 9. Juli 1998 
  Published    1998 
  Keywords    Chalcogenides, Germanium, Copper, Preparation, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1483.pdf 
 Identifier    ZNB-1998-53b-1483 
 Volume    53 
28Author    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 
29Author    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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 Identifier    ZNB-1998-53b-0005 
 Volume    53 
30Author    Sabine Schlecht, Soheila Chitsaz, Bernhard Neumüller, Kurt DehnickeRequires cookie*
 Title    Die Kristallstrukturen des Diphenylphosphinsäureamids, Ph2P(0)NH 2, und seines Cäsiumsalzes [Cs{Ph2P(0)NH}] Crystal Structures of Diphenylphosphinic Acid Amide, Ph-,P(0)NH-, and of its Cesium Salt [Cs{Ph2P(0)NH}]  
 Abstract    The crystal structures of the monoclinic form of Ph2P(0)NH2 and of its cesium salt, [Cs{Ph2P(0)NH}l have been determined by X-ray methods. Ph2P(0)N H 2: Space group P2,/c, Z = 16, lattice dimensions (-80°C): a = 2530.2(3), b = 858.9(2), c = 2135.5(3) pm, ß = 110.78(1)°, R , = 0.055. Diphenylphosphinic acid amide forms dimeric molecules via N-H- • O hydrogen bonds, the dimeric units again are associated via hydrogen bonds to form infinite double chains along the crystallographic c axis. [Cs{Ph2P(0)NH}]: Space group Pccn, Z = 8 , lattice dimensions (-83°C): a = 1262.8(1), b = 2632.3(2), c = 769.1(1) pm , R\ = 0.024. The compound is associated via Cs-O and Cs-N contacts along the crystallographic [001] axis forming a tubular arrangement. There are no hydrogen bonds. 
  Reference    (Z. Naturforsch. 53b, 17—22 [1998]; eingegangen am 3. November 1997) 
  Published    1998 
  Keywords    Phosphinic Acid Amide, Cesium, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0017.pdf 
 Identifier    ZNB-1998-53b-0017 
 Volume    53 
31Author    Wolfgang Jeitschko, HorstA. Mons, Ute Ch, ManfredH. Rodewald, MöllerRequires cookie*
 Title    The Crystal Structure of the Potential Ferroelectric Calcium Rhenate(VI, VII) CanRe4 0 24 and its Relation to the Structure of S rn 0 s40 24  
 Abstract    The title compound was prepared in well-crystallized form by thermal decomposition of Ca5Re20i2. Its structure was determined from single-crystal X-ray diffractometer data: /4 j, a = 1107.0(1), c = 1609.3(1) pm, Z = 4, R -0.056 for 4565 structure factors and 119 variable parameters. The calcium atoms occupy seven different sites with 8, 9, or 10 oxygen neighbors. The two different rhenium atoms are octahedrally coordinated by oxygen atoms with average Re-O distances of 193.1 and 187.7 pm for the six-and seven-valent rhenium atoms, respectively. The compound shows Curie-Weiss behavior with a magnetic moment of n exp = 1.15(±0.10) Pb per Re(VI) atom. The structure is closely related to that of Srn0s4024 which, however, crystallizes in the space group I2la. The difference between the two structures arises through the higher coordination numbers of the strontium atoms. It is suggested that at high temperature both compounds crystallize in the common higher symmetry space group I4\/a. Since CanRe4024 crystallizes in the pyroelectric class 4 this compound is expected to be ferroelectric. 
  Reference    (Z. Naturforsch. 53b, 31—36 [1998]; received October 17 1997) 
  Published    1998 
  Keywords    Crystal Structure, Ferroelectrics, Mixed Valence, Rhenates, Perrhenates 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0031.pdf 
 Identifier    ZNB-1998-53b-0031 
 Volume    53 
32Author    Hk Wulff, Müller-BuschbaumRequires cookie*
 Title    Zur Kristallchemie der Kupfer(II)-ZinkteIlurate Cu5 Zn4Te3 0 18  
 Abstract    Cuj^Znj^TeOg, mit einer Notiz über Cul95Co1?5T e06 On the Crystal Chemistry of the Copper(II) Zinc Tellurates Cu5Zn4Te30 ,8 and Cu, 5Zn, 5Te06 with a Note on Cu, 5Co, 5Te06 L. Single crystals of Cu5Zn4Te30 , 8 (I), Cu, 5Zn, 5Te06 (II) and Cu, 5Co, 5Te06 (III) have been prepared and investigated by X-ray work. The structure of (I) was solved in the monoclinic space group C^-C2, a = 14.834(2), b = 8.801(1), c = 10.375(2) Ä, ß = 93.27(2)°, Z = 4. (II) and (III) crystallize with cubic symmetry, space group Th-Ia3, a{U) = 9.557(1), a(III) = 9.570(1) Ä, Z = 8. (I) shows a complicated structure formed by Te06 octahedra isolated from each other, Zn20 6 double tetrahedra and Zn20 8 double square pyramids. These polyhedra are incorporated into a network of edge and corner connected stretched C u06 octahedra. (II) and (III) are isotypic to Cu3T e06 and have a (Cu/M)30 6 octahedra network, statistically occupied by Cu2+ and Zn2+ or Cu_+ and Co2+. 
  Reference    (Z. Naturforsch. 53b, 53—57 [1998]; eingegangen am 27. Oktober 1997) 
  Published    1998 
  Keywords    Copper, Zinc, Cobalt, Tellurate, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0053.pdf 
 Identifier    ZNB-1998-53b-0053 
 Volume    53 
33Author    Karl-Friedrich Tebbe, Theo Gilles, Bernhard RadkeRequires cookie*
 Title    Untersuchungen an Polyhalogeniden  
 Abstract    , XXXIII [1] Polyiodide des Nickelhexamminkomplexes: Nickelhexamminbistriiodid [Ni(NH3)6](I3) 2 und Nickelhexamminbispentaiodid [Ni(NH3)6 ] (I5)2 Studies of Polyhalides, 33 [11 Polyiodides of the Nickel Hexammine Complex: Nickelhexammine Bistriiodide [Ni(NH3)6](I3)2 and Nickelhexammine Bispentaiodide [Ni(NH3)6l(I5) The compounds [Ni(NH3)6 ](I3) 2 and [Ni(NH3)6 ](I5) 2 have been prepared by the reaction of stoichiometric amounts of [Ni(NH3)6 ]Cl2, KI, and I2 in water. The already known triiodide crystallizes in the monoclinic space group C2/c with a = 1541,0(10), b = 1521.6(8), c = 876.1 (7) pm, ß = 101.44(6)° and Z = 4. The new pentaiodide crystallizes in the monoclinic space group P2,/n with a = 899.6(4), b = 1681.6(5), c = 946.8(7) pm, ß = 110.90(5)° and Z = 2. Both compounds contain nearly octahedral cations [Ni(NH3)6]2+ and simultaneously a linear and a bent triiodide ion I3_ with nearly equal bond lengths or a unsymmetrical V-shaped pentaiodide ion I5_ which is lined up to a new type of pentaiodide chain. 
  Reference    (Z. Naturforsch. 53b, 87—92 [1998]; eingegangen am 25. September 1997) 
  Published    1998 
  Keywords    Polyiodide, Triiodide, Pentaiodide, Nickel Hexammine Complex, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0087.pdf 
 Identifier    ZNB-1998-53b-0087 
 Volume    53 
34Author    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 
35Author    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 
36Author    Dirk Steinbom, Olaf Gravenhorst, Henrik Junicke, FrankW. HeinemannRequires cookie*
 Title    Synthese und Charakterisierung von kronenetherstabilisierten Platin(IV)- Komplexen mit Aminosäureliganden Synthesis and Characterization of Amino Acid Complexes of Platinum(IV) Stabilized by Crown Ethers  
 Abstract    Crown ether complexed pentachloro(aqua)platinic acid, (H30)[PtCl5(H20)]-2(18-cr-6) • 6H20 (1) reacts with glycine, L-alanine, and DL-2-aminobutyric acid to give ds-[PtCl4(0-glyH)(H20)](1 8 -cr-6)H 20 (4a)1 and ds-[PtCl4(0-amacH)(H2O)](18-cr-6) (amacH = alaH 4b, abuH 4c), respectively, as well as (amacH2)2[PtCl6]-2(18-cr-6) (amacH = glyH 5a, alaH 5b, abuH 5c). The crown ether complexed hexachloroplatinic acid, (H30) 2[PtCl6]-2(18-cr-6) (2), reacts with glycine to afford (glyH2)[PtCl4(yV,0-gly)]-2(18-cr-6)1.25H20 (6). The structures of 4b and 6 were determined by X-ray diffraction. The alanine ligand in 4b is a zwitterion that is coordinated to platinum by one oxygen atom of the carboxylate group only. The other oxygen atom is engaged in a strong hydrogen bond to the ds-coordinated aqua ligand. The glycinato ligand in 6 is /V,(9-coordinated at platinum forming an anion [PtCl4(/V,0-gly)]_ . The other oxygen atom of the carboxylate group is involved in a strong hydrogen bridge to the cation (glyH2)+. In both complexes hydrogen bridges are formed between the -N+H3 and -NH2 groups of the amino acid ligands and the oxygen atoms of the crown ether molecules. 1 Abbreviations: amacH = amino acid, glyH = glycine, alaH = L-alanine, abuH = DL-2-amino-butyric acid. 
  Reference    Z. Naturforsch. 53b, 581—586 (1998); eingegangen am 16. Januar 1998 
  Published    1998 
  Keywords    Platinum(IV) Complexes, Crown Ethers, Amino Acids, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0581.pdf 
 Identifier    ZNB-1998-53b-0581 
 Volume    53 
37Author    JuliaA. Manskayaa, KonstantinV. Domasevitcha ', VeraV. Ponomareva2, Joachim Sielerb, VolodimirN. Kokozay2Requires cookie*
 Title    Crystal Engineering towards Design of Macrocyclic Coordination Compounds: Crystal Structure of Rubidium Tetrachloro-and Tetracyanoaurate(III) Complexes with 18-Crown-6  
 Abstract    The new macrocyclic complexes of composition Rb(18-crown-6)AuX4 (X = Cl (1) and CN (2)) have been prepared and characterized by X-ray crystallography (1: monoclinic, space group P2\/n, with a = 8.747(1), b = 8.366(1), c = 15.404(1) Ä; ß = 104.37(1)°, V = 1092.0(3) A , Z = 2; final R 1 =0.025 for 2030 independent reflections used; 2: monoclinic, space group P2\/c, with a = 14.765(3), 6 = 17.134(3), c = 8.855(2) k \ ß = 90.20(1)°, V = 2240.2(8) Ä3, Z = 4; final R 1 = 0.080 for 2034 independent reflections used). Both structures consist of Rb(18-crown-6)+ cations (A) and complex aurate(III) anions AuX4_ (B). Complex 1 has a linear polymeric array -A-B-A-B-(Rb-Cl 3.604(3), 3.654(3) Ä) with the rubidium ions disordered 0.276(2) A above and below the crown ether plane (Rb-O 2.819(5)-2.884(5) A, av. 2.846(5) A). The positioning of the rubidium atom away from the center of the 18-crown-6 is effected by the packing of the Rb(18-crown-6)+ and AuCU-moieties, and by the resemblance in the charge and symmetry of the cationic and anionic parts of the structure. Complex 2 has a zig-zag polymeric array -A-B-A-B-(Rb-N 2.92(2), 2.94(1) A) with orthogonal disposition of Rb(18-crown-6)+ and Au(CN)4-planes. The rubidium atom is situated 0.90(2) A above the mean plane of the macrocyclic oxygen atoms (Rb-O 2.93(5)-3.15(4) A) and adopts a typical "sunrise coordination". 
  Reference    Z. Naturforsch. 53b, 683—688 (1998); received January 5 1998 
  Published    1998 
  Keywords    18-Crown-6, Rubidium Macrocyclic Complexes, Gold(III), Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0683.pdf 
 Identifier    ZNB-1998-53b-0683 
 Volume    53 
38Author    Wolfgang Banße, Jana Fliegner, Stefan Sawusch, Uwe Schilde, Erhard UhlemannRequires cookie*
 Title    Dioxomolybdän(VI)-Komplexe mit dreizähnigen diaciden Liganden Dioxomolybdenum(VI) Complexes with Tridentate Diacidic Ligands  
 Abstract    Dioxomolybdenum(VI) complexes have been synthesized by ligand exchange reactions o f M o(CO)6, M o(NO)2(acac)2 and M o 0 2(acac)2 with tridentate diacidic ligands. X-ray structure analyses were performed on single crystals. The complexes salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (lb) and 2,2'-dihydroxy-azobenzenato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2) are isomorphous. In all chelates the Mo atom is in a distorted octahedral environment. Structural data: Salicylaldehyde-2-hydroxyanilato(2-)-tetrahydrofurane-dioxomolybdenum (VI) (la): a = 23.381(6) Ä, b = 6.756(2) A, c = 28.380(8) A, ß = 124.47(2)°; Salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum (VI) (lb): a = 9.4208(14) A, b = 30.550(5) A, c = 10.461(2) Ä, ß = 111.005(17)°; 2,2'-Dihydroxy-azobenzenato(2-o)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2): a = 9.392(2) A, b = 31.012(13) A, c = 10.350(2) Ä, /3 = 110.968(17)°; Salicylaldehyde-salicylhydrazonato(2-0)-triphenylphosphaneoxide-dioxomolybdenum(VI) (3): a = 9.321(2) A, b = 12.048(2) A, c — 13.858(3) A, a = 101.90(2)°, ß = 94.94(2)°, 7 = 105.479(17)°. 
  Reference    Z. Naturforsch. 53b, 689—693 (1998); eingegangen am 6. März 1998 
  Published    1998 
  Keywords    Ligand Exchange Reactions, Dioxomolybdenum(VI) Complexes, Tridentate Diacidic Ligands, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0689.pdf 
 Identifier    ZNB-1998-53b-0689 
 Volume    53 
39Author    Abdel-Fattah Shihada, Frank WellerbRequires cookie*
 Title    Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2C lSn02PMe2  
 Abstract    Diethylchlorotin dimethylphosphinate has been synthesized by treating (E tiC lS n^O with H02PMe2 in toluene. Single crystal X-ray analysis shows that Ü 2PM e2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The S n-C l bond lies on a C2 axis of symmetry in the (C2V) OCClSnCO unit. Et2ClSn02PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, /5 = 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSn0 2 PMe2 are assigned and the mass spectrum is reported and discussed. 
  Reference    Z. Naturforsch. 53b, 699—703 (1998); received December 29 1997 
  Published    1998 
  Keywords    Crystal Structure, IR Data, Mass Spectroscopic Data, Diethylchlorotin Dimethylphosphinate 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0699.pdf 
 Identifier    ZNB-1998-53b-0699 
 Volume    53 
40Author    H. Ans Bock, N.Orbert Nagel, Professor HeinzRequires cookie*
 Title    Wechselwirkungen in Molekülkristallen, 143 [1]. ortho-Benzol-Derivate mit ineinander verzahnten Chlormethyl-und Methylamino-Substituenten: Strukturen und Rotationsenthalpie-Hyperflächen  
 Abstract    Interactions in M olecular Crystals, 143 [1]. orr/io-B enzene Derivatives w ith M eshed C ogw heel C hlorom ethyl and M ethylam ino Substituents: Structures and R otation Enthalpy H ypersurfaces Facets of molecular dynamics in organic compounds such as coupled rotations of adjacent substituents are advantageously discussed based on structural data. Within this context, crystal structures of spatially overcrowded ortho-disubstituted benzene derivatives with chloromethyl or methylamino groups are presented together with semiempirical enthalpy hypersurfaces for the substituent rotation. Both compounds, 1 -trichloromethyl-2-dichloromethyl-benzene as well as l-trimethylammonium-2-dimethylamino-benzene exhibit comparable steric overcrowding and their preferred dynamics are predicted to be dominated by the rotation of the threefold substituted group during an approximate standstill of the twofold substituted, mirror-symmetric one. According to known solid state NMR measurements as well as to atom/atom-potential model calculations for the pentachloro orf/zo-xylene derivative, this molecular dynamic mode is still active in the crystal. Dreizählige molekulare Zahnrad-Systeme Bei der zahnradartigen, 
  Reference    Z. Naturforsch. 53b, 792—804 (1998); eingegangen am 10. März 1998 
  Published    1998 
  Keywords    ortho-Benzene Derivatives, Meshed Cogwheel Substituents, Crystal Structure, Rotation Enthalpy Hypersurfaces 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0792.pdf 
 Identifier    ZNB-1998-53b-0792 
 Volume    53 
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