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241Author    Kai Landskron, Stefan Horstmann, Wolfgang SchnickRequires cookie*
 Title    Neue Tetraaminophosphonium-Salze durch Anionenaustausch in flüssigem Ammoniak Novel Tetraaminophosphonium Salts by Anion Exchange in Liquid Ammonia  
 Abstract    [P(NH2)4]Br and [P(NH2)41[N 03] have been prepared by anion exchange in liquid ammonia. Single crystals of [P(NH2)4]Br were obtained from an acetonitrile solution in a tempera­ ture gradient between 60 °C and room temperature while attempts to grow single crystals of [P(NH2)4][N 0 3] yielded [P(NH2)4][N 0 3](O P(N H 2)3). Both crystal structures were determined by single crystal X-ray methods at room temperature ([P(NH-))4]Br: P4/nbm, a = 809.2(1), c = 468.1(1) pm, Z = 2, R \ = 0.042, wR2 = 0.077; [P(NH2)4][NÖ3](OP(NH2)3): Pna2,, Z = 4, a = 1023.4(1), b = 1704.7(1), c = 618.0(1) pm, R \ =0.025', wR2 = 0.067. In the solid [P(NH2)4]Br forms a tetragonally distorted variant of the CsCl type of structure. [P(NH2)4][N 0 3](0P (N H 2)3) consists of [P(NH2)4]+cations, [N 0 3]_ anions, and OP(NH2)3 molecules which are interconnec­ ted by a complex system of hydrogen bonds. 
  Reference    Z. Naturforsch. 54b, 1019—1026 (1999); eingegangen am 12. April 1999 
  Published    1999 
  Keywords    Phosphorus, Ion Exchange, Liquid Ammonia, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1019.pdf 
 Identifier    ZNB-1999-54b-1019 
 Volume    54 
242Author    *. Sonderdruckanforderungen, ProfK. Dr, DehnickeRequires cookie*
 Title    D ie Kristallstruktur von Bis(bromo  
 Abstract    -triphenyl)arsen(V)-hexabromo-tellurat(IV), [Ph3A sB r]2[TeBr6] Crystal Structure o f B is(brom otriphenyl)-arsen ic(V)-h exab rom otellu rate(IV), [Ph3A sB r]2[TeBr6] S oheila Chitsaz, Bernhard N eum üller, Kurt D eh nick e* Yellow-orange single crystals of [Ph3AsBr]2[TeBr6] have been prepared from satu­ rated solutions of Ph3AsBr2 and TeBr4 in aceto­ nitrile and characterized by a crystal structure de­ term ination. Space group R3c, Z = 12, lattice di­ mensions at -7 0 °C: a = b = 1337.9(2), c = 7953.8(4) pm, R = 0.0691. The structure consists of discrete ions [Ph3A sBr]+ and nearly perfectly octahedral [TeBr6]2-. 
  Reference    Z. Naturforsch. 54b, 1092—1094 (1999); eingegangen am 28. Mai 1999 
  Published    1999 
  Keywords    Arsenic, Tellurium, Bromo Complex, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1092_n.pdf 
 Identifier    ZNB-1999-54b-1092_n 
 Volume    54 
243Author    Santiago Garcia-Yustea, KonradW. Hellmanna, LutzH. Gadeb, IanJ. Scowenc, Mary McpartlincRequires cookie*
 Title    Bis[l,3-bis(diphenylmethylsilylamido)propane]zirconium: A Spirocyclic Complex Containing a Sterically Demanding Chelating Amido Ligand  
 Abstract    Lithiation of the diamine CH2(CH2NHSiMePh2)2 using »-butyl lithium and subsequent reaction with zirconium tetrachloride yielded the bis(chelate)-amidozirconium complex [Zr{CH2(CH2NSiMePli2)2 }2]-The spirocyclic molecule has a distorted tetrahedral coordi­ nation at the zirconium centre with overall C2 symmetry broken only by the relative orientation of four phenyl rings. The bulky diphenylmethylsilyl substituents at the amido-N functions as well as the ligand backbone sterically protect the metal centre and render it inert towards conproportionation with zirconium chloride. 
  Reference    Z. Naturforsch. 54b, 1260—1264 (1999); received July 2 1999 
  Published    1999 
  Keywords    Silylamides, Zirconium Amide, Chelate Ligands, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1260.pdf 
 Identifier    ZNB-1999-54b-1260 
 Volume    54 
244Author    Birgit Fehrmann, Wolfgang JeitschkoRequires cookie*
 Title    The Intermetallic Compounds GdRe2Al10 and TbRe2Al10, Crystallizing with a Stacking Variant of the YbFe2Al10 Type Structure  
 Abstract    The new compounds GdReaAlio and TbRe.Alio were obtained in well-crystallized form by reaction of the elemental components with an excess of aluminum after dissolving the matrix in hydrochloric acid. They crystallize with a new structure type which has been determined for TbReiAlio from single-crystal X-ray data: Cmcm, a = 932.2(1),/?= 1030.4(1),c= 1803.2(3)pm, Z = 8, R = 0.031 for 1159 structure factors and 77 variable parameters. Of the two terbium sites, one does not have full occupancy with terbium, however, it may have mixed Tb/Al occupancy. The resulting compositions are Tbo.948(5>Re2Alio or Tbo.936(3)Re:Alio.o64(3), respectively. The terbium atoms are coordinated by 4 Re and 16 Al atoms. The rhenium atoms are situated in distorted icosahedra formed by 2 Tb and 10 Al atoms. The nine different aluminum atoms have between 12 and 14 neighbors (1 or 2 Tb, 2 Re, and between 8 and 11 Al atoms). The structure may be viewed as consisting of two kinds of alternating layers. One of these is puckered, hexagonal close packed, with a mesh content of 4ReAl3; the other is planar and less densely packed. It has the mesh content 2TbAl4. The same kinds of atomic layers have been found in the structures of YbFe2Alio and LuRe2Alio. Thus, the three structure types may be considered as stacking variants of each other. The tetragonal CaC^Alio (ordered ThMni2) type structure also belongs to this structural family, although the CaAl4 layers somewhat differ from the layers TbAl4, YbAl4, and LuA14. 
  Reference    Z. Naturforsch. 54b, 1277—1282 (1999); received May 27 1999 
  Published    1999 
  Keywords    Intermetallic Compounds, Crystal Structure, Close Packed Layers 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1277.pdf 
 Identifier    ZNB-1999-54b-1277 
 Volume    54 
245Author    Qianfeng Zhanga, Jinxi Chena, Maochun Hongb, Xinquan Xina, Hoong-Kun FuncRequires cookie*
 Title    Crystal and Molecular Structure of the Copper(I)-thiolate-selenide Complex [Ph4P][Cu(SeS2CNC4H8)(S2CN2C4H8)] with an Unusual Se-S Bond  
 Abstract    Reaction of a DMF solution of Cu(S^CNC4 H8) with [Ph4 P]2 [WSe4 ] affords [Ph4 P b[W Se4 -(CuS2CNC4H8)3 ] (1) and [Ph4P][Cu(SeS2 CNC4 H8)(S2 CN2 C4 H 8)] (2) in which a Se atom from the decomposition of the W Se4 2~ anion has reacted with the pyrrolidyldithiocarbamate (C4 H8dtc) ligand anion to form the new ligand anion SeSiC N C +H s'. Complex 2 crystallizes with four formula units in the monoclinic space group P2\/c in a cell of dimensions a = 10.5824(2), b = 18.7575(3), c = 18.3268(4) A and ß = 109.0980(10)°. 6055 independent reflections above background were measured with a diffractometer and the structure was re­ fined anisotropically to R =0.073. The anion contains a three-coordinated copper(I) atom. The C4 H8 dtcö ligand is bonded to the Cu+ cation in a terminal fashion, while SeS2 CNC4 H8~ chelates the Cu+ cation. The Se-S bond length is 2.231 (4) A. 
  Reference    Z. Naturforsch. 54b, 1313—1317 (1999); received April 4 1999 
  Published    1999 
  Keywords    Crystal Structure, Copper Complex, Selenium Complex, Thiolate Ligand 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1313.pdf 
 Identifier    ZNB-1999-54b-1313 
 Volume    54 
246Author    Michael Becker, Martin Jansen, Martin Jansen Heisenbergstraße, D-70596, Stuttgart Sonderdruckanforderungen, Prof Dr, Martin JansenRequires cookie*
 Title    Darstellung und Charakterisierung von Rubidiumhydrogencyanamid Synthesis and Characterization of Rubidium Hydrogen Cyanamide  
 Abstract    The synthesis of RbHCN2 was carried out by reaction of cyanamide with rubidium amide in liquid ammonia. The crystal structure has been determinedo by x-ray powder methods (orthor-hombic, P2,2,2,, a = 7.299(1), b = 9.435(1), c = 9.420(1) Ä; Z = 8). The anion is slightly bent (174°) and exhibits two different bond lengths (C-N: 1.17, HN-C: 1.31 A). 
  Reference    Z. Naturforsch. 54b, 1375—1378 (1999); eingegangen am 26. Juli 1999 
  Published    1999 
  Keywords    Rubidium Hydrogen Cyanamide, Synthesis, Crystal Structure, IR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1375.pdf 
 Identifier    ZNB-1999-54b-1375 
 Volume    54 
247Author    Stefan DickRequires cookie*
 Title    Uber die Struktur von synthetischem Tinsleyit K[A12 (P04)2(0H)(H20)]H 20 The Structure of Synthetic Tinsleyite K[A12 (P0 4)2 (0 H)(H2 0 )] H20  
 Abstract    Synthetic tinsleyite KfAhCPO-ibCOHXFTO^TTO has been obtained by the reaction of gibb-site with a potassium-phosphate solution of pH = 7 at 423 K within five days. A single crystal X-ray structure analysis has shown that synthetic tinsleyite is isotypic with the mineral leucophosphite K[Fe2(P0 4)2(0 H)(H20)] H 20. Crystal data: monoclinic space group P2\/n, a = 949.9(2), b = 950.3(2), c = 953,5(2) pm, ß = 103,26(3)°, Z = 4. The structure of tinsleyite consists of tetranuclear A I4O 2 units formed by a central pair of edge sharing A1Ü6 octahedra, to which two additional A1C>6 octahedra are attached sharing corners. These units are crosslinked by phosphate ions to a three dimensional framework structure with tunnels along [010], occupied by potassium cations. While one type of water molecules is attached to Al, a second type is fixed in the structure by hydrogen bonds only. As a consequence two steps for thermal loss of water at 341 K and 471 K are observed. 
  Reference    Z. Naturforsch. 54b, 1385—1390 (1999); eingegangen am 15. Juli 1999 
  Published    1999 
  Keywords    Crystal Structure, Phosphate Mineral, Tinsleyite, Leucophosphite 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1385.pdf 
 Identifier    ZNB-1999-54b-1385 
 Volume    54 
248Author    Marcus Sigl, Annette Schier, Hubert SchmidbaurRequires cookie*
 Title    Bis[(2-diphenyIphosphino)phenyl]phenylphosphine as an Inflexible Tridentate Ligand for Indium Trichloride  
 Abstract    Anhydrous indium trichloride reacts with [2-(Ph2P)C6H4]2PPh (TP) in the molar ratio 2:1 to give an ionic complex [(TP)InCl2]+ InC L-in almost quantitative yield. The structure of the product has been determined by a single crystal X-ray diffraction study. In the cation the TP molecule acts only as a bidentate ligand via its two terminal phosphorus atoms [In-Pl 2.5956(8), In-P2 2.5799o (7) A], Although the central phosphorus atom is also rather close to the metal atom [2.8259(8) A], the In-P3 interaction is inefficient because of an adverse orientation of the lone pair of electrons at P3 owing to the steric inflexibility of the ligand. Accordingly, the 11P N M R spectra of the compound in C D 2CI2 show large contact shifts and quadrupole broadening only for the signals of the two terminal phosphorus atoms, whereas the lines of the central phosphorus atom are less shifted and well resolved (A B2 spin system at -60°C). 
  Reference    Z. Naturforsch. 54b, 1417—1419 (1999); received September 15 1999 
  Published    1999 
  Keywords    Indium Trichloride, Tridentate Phosphine, Ligand Inflexibility, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1417.pdf 
 Identifier    ZNB-1999-54b-1417 
 Volume    54 
249Author    Wolfgang Jeitschko, HorstA. Mons, Ute Ch, RodewaldRequires cookie*
 Title    Preparation and Crystal Structure of the Calcium Rhenate(VI, VII) Ca5Re30 15.x  
 Abstract    The title compound was prepared by reaction of elemental calcium with the calcium metaper-rhenate Ca(ReC>4)2. Its crystal structure was determined from single-crystal X-ray data: Amm2, a = 560.31 (5)pm, b = 1572.4(1)pm, c = 719.91 (6)pm ,Z = 2 ,R = 0.033 for 930 structure factors and 46 variable parameters. The calcium atoms occupy three atomic sites, all with seven oxygen neighbors. Of the two different rhenium atoms one has square-pyramidal oxygen coordination with an average oxidation number +6.25. The other rhenium site (oxidation number +7) was refined as a split position with trigonal-bipyramidal (75%) and tetrahedral oxygen coordination (25%). One oxygen site remains unoccupied, whenever the tetrahedral rhenium site is occupied, resulting in the composition Ca5Re3 0 i4.75. A test for superconductivity of this black compound down to 1.5 K was negative. 
  Reference    Z. Naturforsch. 54b, 1483—1488 (1999); received August 16 1999 
  Published    1999 
  Keywords    Crystal Structure, Mixed Valence, Rhenates, Perrhenates 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1483.pdf 
 Identifier    ZNB-1999-54b-1483 
 Volume    54 
250Author    KurtO. Klepp, Ferdinand Fabian, *. Sonderdruckanforderungen, Prof Kurt, O. KleppRequires cookie*
 Title    Darstellung und Kristallstruktur von Rb6Sn2S7 New Chalcogenometallates with Binuclear Anions, I: Preparation and Crystal Structure of Rb6Sn2S7  
 Abstract    Colorless crystals of the new thiostannate Rb6Sn2S7 were obtained by reacting a stoichio­ metric melt of Rb2S, Sn and S at 700°C. The compound is orthorhombic, oP60, s.g. f '2,2,2, (No. 19) with a = 9.982(4), b = 13.45(1), c = 15.20(1) A; Z = 4. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.043 (1380 Fo's, 137 variables). The crystal structure contains dimeric anions, [Sn2S7]2 -, which are built up by slightly distorted SnS4 tetrahedra sharing a common sulfur atom. The mean Sn-S bond length calculates as 2.384 Ä, the bond angle on the bridging S is 110.4°. The structure contains six independent Rb-cations which are coordinated to 5-6 sulfur atoms in irregular configurations. Neue Chalkogenometallate mit binuklearen Anionen, I: 
  Reference    Z. Naturforsch. 54b, 1505—1509 (1999); eingegangen am 13. September 1999 
  Published    1999 
  Keywords    Crystal Structure, Chalcogenides, Thiostannates, Rubidium, Tin, Sulfur 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1505.pdf 
 Identifier    ZNB-1999-54b-1505 
 Volume    54 
251Author    M. Karl, G. Seybert, W. Massa, K. DehnickeRequires cookie*
 Title    Die Kristallstruktur von [YbCl2(THF)5]+[WOCl4(TH F)]- Crystal Structure of [YbCl2(THF)5]+ [WOCl4(THF)]  
 Abstract    Blue moisture sensitive single crystals of [YbCl2(THF)5]+ [WOCl4(THF)]-were obtained as a by-product from the reaction of the ytter­ bium trisamide Yb[N(SiMe3)2]3 with tungsten he-xachloride in THF solution. The crystals were sui­ table for an X-ray crystal structure determination. Space group P2/c, Z = 2, lattice dimensions at 
  Reference    Z. Naturforsch. 54b, 1609—1610 (1999); eingegangen am 23. August 1999 
  Published    1999 
  Keywords    Ytterbium, Chloro-THF-Complex, Tungsten, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1609_n.pdf 
 Identifier    ZNB-1999-54b-1609_n 
 Volume    54 
252Author    Bernhard Neumüller, Soheila Chitsaz, Kurt DehnickeRequires cookie*
 Title    Die Kristallstrukturen von Ph3AsCI2 und /?-Ph3AsBr2 Crystal Structures of Ph3AsCl2 and ß-Ph3AsBr2  
 Abstract    Colourless single crystals of Ph3A sC l2 as well as of /?-Ph3AsBr2 were obtained from acetonitrile solutions and were suitable for X-ray structure determinations. Ph3AsCl2: Space group P212121, Z = 4, lattice dimensions at -90 °C: a = 1247.9(2), b = 
  Reference    Z. Naturforsch. 54b, 1611—1614 (1999); eingegangen am 23. August 1999 
  Published    1999 
  Keywords    Arsenic, Triphenylarsenic Dichloride, Triphenylarsenic Dibromide, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1611_n.pdf 
 Identifier    ZNB-1999-54b-1611_n 
 Volume    54 
253Author    M. Ichaela, W. Ilhelm, W. Olfgang Saak, H. Enry StrasdeitRequires cookie*
 Title    Phenylmercury Chloride: Its Single-Crystal X-Ray Structure and Some Aspects of its Biological Chemistry  
 Abstract    A single crystal of phenylmercury chloride (PhHgCl) was obtained by serendipity from a solution of diphenylmercury (HgPh2) and dihydrolipoic acid in tetrahydrofuran / carbon tetrachloride. The crystal structure of PhHgCl is pseudotetragonal. It is best described in the orthorhombic space group Cmma with a = 6.856(1), b = 6.882(1), c = 14.309(2) A (at 193 K), and Z = 4. The Cl-Hg-C moiety of the PhHgCl moleculeois exactly linear. The bond lengths at the Hg atom are Hg-Cl 2.345(2) and Hg-C 2.044(9) Ä. In the crystal, the molecules are arranged in double layers parallel to the a,b plane. In a model medium for the gastric juice (0.1 M DC1 in D 20 / [Dg]dioxan, 37 °C), HgPh2 reacts to form PhHgCl. HgCl2, which would result from complete dearylation, cannot be isolated from the reaction mixture. However, it appears that a small equilibrium concentration of HgCl2 may be present, because on addition of 1,4,7-trithiacyclononane (ttcn) and diethyl ether, the dichloride can be trapped as solid [Hg(ttcn)2][HgCl4]. We estimate that after oral uptake of HgPh2 20 -90% are transformed into PhHgCl in the stomach after 30 min. In tro d u ctio n 
  Reference    (Z. Naturforsch. 55b, 35—38 [2000]; received October 18 1999) 
  Published    2000 
  Keywords    Acidolysis, Bioinorganic Chemistry, Crystal Structure, Mercury, Organomercury Compounds 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0035.pdf 
 Identifier    ZNB-2000-55b-0035 
 Volume    55 
254Author    K. Urt, O. KleppRequires cookie*
 Title    Preparation and Crystal Structure of Na4TiSe4. A Selenotitanate with Discrete Tetrahedral Anions  
 Abstract    Red crystals of Na4TiSe4 were obtained by reacting an intimate mixture of Na2Se, Ti and Se at 750°C. Na4TiSe4 is monoclinic, space group I2/a with a = 24.027(6), b = 7.346(4), c = 21.572(6) A, (3 = 104.52(2)°, Z = 16. Its crystal structure was determined from diffractometer data (AgK a-radiation) and refined to a conventional R of 0.036 for 2673 F0's and 158 variables. The crystal structure is of a new type, characterized by the presence of discrete tetrahedral complex anions, [TiSe,*]4" , which are arranged in slabs parallel to (100). The average Ti-Se bond length is 2.385(1) A. The Na+ cations are in different chalcogen environments with distorted octahedral, square pyramidal or planar configurations, respectively. 
  Reference    (Z. Naturforsch. 55b, 39—44 [2000]; received September 28 1999) 
  Published    2000 
  Keywords    Crystal Structure, Chalcogenides, Titanium, Sodium, Selenium 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0039.pdf 
 Identifier    ZNB-2000-55b-0039 
 Volume    55 
255Author    M. Elanie Piilm, Joachim Becht, R. Einhold TackeRequires cookie*
 Title    Singly Charged A6Si-Silicate Anions with an Si¥5C Skeleton: Syntheses and Crystal Structure Analyses of the Ionic Hexacoordinate Silicon Compounds [Me3NH][F5SiCH2N M e2H ]H 20 and [Me3NH][F5SiCH2NMe3] H2 0  
 Abstract    The zwitterionic A^S/'-tetrafluorosilicates F4SiCH 2N M e2H (1) and F4SiCH2NM e3 (2) behave as Lewis acids and react with [Me3NH]F (molar ratio 1:1) in aqueous solution to yield the ionic A657-pentafluorosilicates [Me3NH][F5SiCH2N M e2H] (3) and [Me3NH][F5SiCH2N M e3l (4), respectively. These hexacoordinate silicon compounds contain singly charged A6S/-silicate anions ([F.sSiCHiNM eiH]-, [F5SiCH2NM e3]-) with an S/F 5 C skeleton. Compounds 3 and 4 were isolated as the crystalline hydrates 3 H 20 (yield 80%) and 4 H 20 (yield 82%) which were structurally characterized by single-crystal X-ray diffraction. The ^/-coordination polyhedra in the crystals of 3 H 20 and 4 H20 are slightly distorted octahedra. 
  Reference    (Z. Naturforsch. 55b, 60—64 [2000]; received October 5 1999) 
  Published    2000 
  Keywords    Pentacoordinate Silicon, Hexacoordinate Silicon, Lewis Acid, Crystal Structure 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0060.pdf 
 Identifier    ZNB-2000-55b-0060 
 Volume    55 
256Author    Henri Brunner, M. Arkus, N. Iem Etz, M. Anfred ZabelRequires cookie*
 Title    Optisch aktive Ubergangsmetall-Komplexe, 122 [1]. Synthese von Palladium(II)-Schiff-Base-Komplexen -intramolekulare Wechselwirkungen O ptically Active Transition M etal C om plexes, 122 [1], Synthesis of Palladium (II) Com plexes w ith Schiff B ase Ligands -Intram olecular Interactions  
 Abstract    Imines of salicylaldehyde and 2,6-diformyl-p-cresol have been used as ligands in palla­ d iu m ^) complexes. Enantiomerically pure ligands give enantiomerically pure complexes, racemic ligands give racemates and meso-forms. Differences between the respective isomers of the ligands within the complexes and between the diastereomers of the complexes were investigated. Crystal structure analyses established the trans configuration at the metal center. 
  Reference    Z. Naturforsch. 55b, 145—154 (2000); eingegangen am 25. Oktober 1999 
  Published    2000 
  Keywords    Schiff Bases, Palladium(II) Complexes, Diastereomers, Crystal Structure 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0145.pdf 
 Identifier    ZNB-2000-55b-0145 
 Volume    55 
257Author    C. Bender, D. W. Ulff-M, H. Older, F. Vogt, M. M. Ritschl, EiselRequires cookie*
 Title    Synthese und Kristallstruktur des Bromdifluormethyl-triphenyl- phosphoniumbromids, [(C6H5)3 PCF2Br]+ Br" Synthesis and Crystal Structure o f B rom odifluorom ethyl-triphenylphosphonium Brom ide, [(C6H5)3PC F2Br]+ Br~  
 Abstract    Difluorobromomethyl-triphenylphosphonium bromide [(C6H5)3PCF2Br]+ Br-(1) has been prepared by the reaction of triphenylphosphine with dibromodifluoro-methane in acetonitrile or methylene chloride. The colorless crystals are monoclinic, space group P 2,/n, Z=4, a = 1067.1(2), b = 1488,5(2), c = 1178,2(2) pm, ß = 95,67(3)°. The lattice contains Br~ anions and [(C6H5)3PCF2Br]+ cations with a Br-Br distance of 322,33(11) pm.. For the title compound the results of AM 1, PM 3 ,and MNDO calculations are in good agreement with corresponding values determined by the X-ray analysis only in the case of PM 3. The yellow-red [(C6H5)3PCF2Br]+ Br3~ (2) has been obtained by treating 1 with equimolar quantities of elemental bromine in methylene chloride solution. E inleitung 
  Reference    Z. Naturforsch. 55b, 167—170 (2000); eingegangen am 28. Oktober 1999 
  Published    2000 
  Keywords    Bromodifluoromethyl-triphenylphosphonium Bromide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0167.pdf 
 Identifier    ZNB-2000-55b-0167 
 Volume    55 
258Author    AlfonsoC. Astiñeiras-C, Am, IgnacioS. De L, Cueva -Torregrosab, JosefaM. G Onzález-Pérezb, A. Urora, G. Sicilia-Z, ElenaB. Afrab, A. Ugella-, JuanN. Ltam Iranob, S-G Icló, UtiérrezbRequires cookie*
 Title    Synthesis, Structure and Properties of / > o/j-[(Ar-(2-Hydroxyethyl)- Af'-carboxymethyl-l,2-ethyIenediamine-AyV'-Diacetato)copper(II) Hydrate], {[Cu(Hhedta)] * H20 } n  
 Abstract    The stoichiometric reaction of /V-(2-hydroxyethyl)-1,2-ethylenediamine-/V,/V,7V'-triacetic acid [hbhedta = (H0CH2CH2)(H02CCH2)NC2H4N(CH2C02H)2)] and copper(II) hydroxy-carbo-nate in water yields crystalline samples of /?0/v-{(/V-(2-hydroxyethyl)-/V'-carboxymethyl-l,2-ethylenediamine-./V,./V'-diacetato)copper(II) hydrate}, {[Cu(Hhedta)] TTOjn (I)-The com­ pound was studied by TG analysis (with FT-IR study of the evolved gases), IR, electronic and ESR spectra, magnetic susceptibility data and single crystal X-ray diffraction methods. It crystallises in the orthorhombic system, space group Fdd2 (a = 21.906(2), b = 36.602(4), c = 6.928(1) A, Z = 16, and final R\ = 0.029 for 1554 independent reflections). The Cu(II) atom exhibits a very distorted octahedral coordination (type 4+1 + 1). The Hhedta ligand plays a yV,yV',0,C>',(9"-pentadentate chelating role as well as a O,0'-carboxylate bridging one and has a free /V-carboxymethyl arm. The bridging carboxylate group of the Hhedta ligand leads to polymeric chains {[Cu(Hhedta)] H20}n parallel the c axis. A hydrogen bonding network involves all O-H polar bonds (non-ionised carboxylic and alcoholic hydroxyl groups and water molecules). The structure reveals the preferred formation of a copper(II)-(/V-2-hydroxyethyl-amino) or copper(II)-(ethanolamino) versus a copper(II)-(/V-carboxymethylamino) chelate ring. In tro d u c tio n 
  Reference    Z. Naturforsch. 55b, 171—177 (2000); received October 10 1999 
  Published    2000 
  Keywords    Copper(II) Chelate, Crystal Structure, Amino-polycarboxylates, Ethanolamine 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0171.pdf 
 Identifier    ZNB-2000-55b-0171 
 Volume    55 
259Author    Robert Becker, Wolfgang Brockner, Brigitte EisenmannRequires cookie*
 Title    Kristallstruktur und Schwingungsspektrum des Thallium(I)-Zinn(II)-ortho-Thiophosphates TlSnPS4  
 Abstract    TlSnPS4 crystallizes in the orthorhombic system, space group P na21 (Nr. 33), Z = 4 with the lattice constants a = 1175.8 (5) pm, b = 890.1 (4) pm, c = 663.3 (4) pm. In the structure are sligthly distorted discrete PS4_ anions. The far infrared, infrared and Raman spectrum is assigned on the basis o f P S]-units with C 3v symmetry. According to the DTA data the m elting point for TlSnPS4 is 575 ± 5 °C. The title compound is not moisture sensitive and semi-conducting. 
  Reference    Z. Naturforsch. 42a, 1309—1312 (1987); received Septem ber 15 1987 
  Published    1987 
  Keywords    ortho-Thiophosphate, TlSnPS4, Crystal Structure, Vibration Spectrum 
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 TEI-XML for    default:Reihe_A/42/ZNA-1987-42a-1309.pdf 
 Identifier    ZNA-1987-42a-1309 
 Volume    42 
260Author    J. Pirnat, J. Lužnik, Z. Trontelj, P. K. KadabaRequires cookie*
 Title    Iodine NQR and Phase Transitions in [N(CH 3 ) 4 ] 2 ZnI 4 * a  
 Abstract    Using a superregenerative NQR spectrometer, the temperature dependence of 127 I NQR spectra in [N(CH 3) 4 ] 2 ZnI 4 was measured between 167 and 335 K. The measurements confirm two known structural phase transitions at 219 and 257.5 K. The correspondence between the distinct regions of iodine NQR spectra and the crystal structure is discussed. The relation of [N(CH 3) 4 ] 2 ZnI 4 to the incommensurate family with the general formula X 2 YZ 4 and the high temperature (paraphase) crystal space group D^ (Pmcn) is studied. 
  Reference    Z. Naturforsch. 45a, 349—352 (1990); received August 23 1989 in revised form 25 November 1989 
  Published    1990 
  Keywords    NQR, phase transitions, ferroelectric, crystal structure, displacement modulation 
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 TEI-XML for    default:Reihe_A/45/ZNA-1990-45a-0349.pdf 
 Identifier    ZNA-1990-45a-0349 
 Volume    45