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1Author    A.B M Sham, Rahm An, H. Boiler, K. O. KleppRequires cookie*
 Title    Synthesis and Spectroscopic Investigations of New Linear Heterobimetallic Clusters [Me4N]3[(TOS3 )2Ag] (T = Mo, W). Crystal Structure of [Me4N]3[(MoOS3 )2 Ag]  
 Abstract    Red-brown crystals of a new bis(thiomolybdate) complex [Me4N]3[(MoOS3)2Ag] were formed at room temperature through the reaction of a solution of [Me4N]2[MoOS3] in MeCN with solid AgCN. They are monoclinic, space group P2i/c with unit cell parameters a = 16.662(9), b = 9.464(3), c = 17.890(8) A, /3 = 101.87(2)°, Z = 4. The crystal structure was determined from single crystal diffractometer data (MoKa-radiation) and refined to R = 0.044 (3614 reflections, 236 variable parameters). The structure is characterized by trinuclear complex anions, [(MoOS3)2Ag]3~. According to Weissenberg investigations the homologous tungsten compound is isostructural. The infrared spectrum of the molybdenum complex (KBr powder) shows absorption bands at 884 (vs) and 871 (w) cm-1 (terminal i/(Mo-0)), 483 (vs) cm-1 (terminal i/(Mo-S)), 451 (vs), and 435 (w) cm-1 (bridging i/(Mo-S)). The tungsten complex showed bands at 901 (vs) cm-1 (terminal ^(W-O)), 478 (vs) cm-1 (terminal u(W-S)), and 435 (vs) cm-1 (bridging ^(W-S)). The anionic mass spectra shows molecular ion peaks at m/z 524 and 700 for [(MoOS3)2Ag]_ and [(WOS3)2Ag]~, respectively, as well as peaks for other fragments. 
  Reference    Z. Naturforsch. 55b, 238—242 (2000); received Oktober 10 1999 
  Published    2000 
  Keywords    IR Data, Chalcogenides, Molybdenum, Tungsten 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0238.pdf 
 Identifier    ZNB-2000-55b-0238 
 Volume    55 
2Author    2s4-M Gin2s4, H. Haeuseler, W. CordesRequires cookie*
 Title    Subsolidus Phasenbeziehungen in den Systemen M g G a 2S4-M gC r2S4  
 Abstract    Neue Verbindungen mit Spinell-, Olivin-und ZnIn2S4(IIIa)-Struktur Subsolidus Phase Relationships in the Systems M g G a 2S4-M gC r2S4 and M g G a 2S4-M gIn 2S4 N e w Compounds with Spinei-, O livine-and Zn In 2S4(IIIa)-T y p e Structure The title systems have been investigated on samples quenched at 700, 800 and 1000 °C. Five new compounds have been obtained and characterized by X-ray powder diffraction: Spinel type M gG a02C rl 8S4, two compounds crystallizing in the olivine structure, MgGaCrS4 and M gGaInS4, and two layered materials, M gGaj 5Cra5S4 and M gG aj 5In0.5S4. Lattice para­ meters and phase widths o f the compounds are given. 
  Reference    Z. Naturforsch. 51b, 457—460 (1996); eingegangen am 6. Novem ber 1995 
  Published    1996 
  Keywords    Chalcogenides, Olivine Type Structure, Spinei, Layered Structures 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0457.pdf 
 Identifier    ZNB-1996-51b-0457 
 Volume    51 
3Author    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 
4Author    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 
5Author    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 
6Author    A.B M Shamsur, Rahman, H. Boiler, K. O. KleppRequires cookie*
 Title    Synthesis and Structural Characterization of [Me4N]2[W202(/i-S)(r72-S2)4]*MeCN, a Novel Oxo-thiotungstate(VI)  
 Abstract    Orange red crystals of the new compound [Me4 N]2 [W2 0 2 (^ -S 2)(?/2 -S2)4 ] MeCN were ob­ tained from the reaction of a solution of [Me4 N ]2 [WOS3 ] in MeCN with solid AuCN at room temperature. They are monoclinic, space group P2|//?, with a = 9.264(2), b = 17.736(3), c = 18.742(5) A, ß = 95.19(1)°; Z = 4. The crystal structure was determined from single crystal diffractometer data (M oKa-radiation) and refined to R = 0.050 (2955 reflections, 221 variable parameters). It is characterized by binuclear complex anions [(S2)2 0 WSWO(S2)2 r with close to C2 symmetry. Each metal center is surrounded by two end-on coordinating disulfide groups at distances ranging from 2.37 to 2.42 A which together with a bridging sulfur atom (dw-s = 2.445 A) occupy the equatorial positions of a pentagonal bipyramid whose apices are defined by a terminal oxygen atom (dw -o ~ 1 -725 A) and one sulfur atom of the neighboring component at a distinctly larger distance (dw -s ~ 2.82 A). Infrared spectra of the complex (KBr powder) showed z/(W-O) and i^(W-S) of bridging W-S-W at 931 (vs) and 454 (m) cm -1, respectively, u{ W-S) of the W S2 unit appeared in the range between 465 and 438 crrT 1. The mass spectrum of the anion showed the molecular mass at m/z 6 8 8 for [W2 0 2 S9 ]~ as well as peaks for other fragments. 
  Reference    Z. Naturforsch. 54b, 1318—1322 (1999); received April 19 1999 
  Published    1999 
  Keywords    Crystal Structure, IR Data, Chalcogenides, Complex Sulfides, Tungsten Compounds 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1318.pdf 
 Identifier    ZNB-1999-54b-1318 
 Volume    54