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1999 (1)
1Author    Hans-JoachimD. Rexler3, Ines Starkeb, M. Anuela, G. Rotjahnb, Helmut Reinke3, Erich Kleinpeterb, Hans-JürgenH. Oldt3Requires cookie*
 Title    SbCI3, BiCl3 and Na+ Complexes of Maleonitrile-Dithiacrown Ethers: Synthesis, Crystal Structures and DEP-MS Experiments  
 Abstract    The reactions of MC13 (M = Sb, Bi) with maleonitrile-dithia-15-crown-5 (mn-15S20 3) and maleonitrile-dithia-18-crown-6 (mn-18S20 4) in MeCN yielded the complexes [MCl3(mn-15S20 3)] {M = S b (l), Bi(2)} and [MCl3(mn-18S20 4)] {M = Sb(3), Bi(4)}, respec­ tively. The pyramidal MC13 units are coordinated very weakly to the three oxygen and two sulphur donor atoms of mn-15S20 3 in 1 and 2, and to the four oxygen donor atoms o f mn-18S20 4 in 3 and 4. Both mn-15S20 3 com plexes, 1 and 2, crystallize isotypically in the m ono­ clinic space group P2(\)ln with four formula units per unit cell, while the isotypic mn-18S20 4 complexes, 3 and 4, are triclinic, space group P-1, with two formula units per unit cell. In the SbCl3 complexes, 1 and 3, the mean contact distances between the Sb centres and the macro-cyclic donor atoms are longer than the corresponding distances in their isostructural BiCl3 analogues, 2 and 4, which may reflect a stereochem ical activity of the Sb,n lone pair. Under the conditions of DEP-M S experim ents with 1 and 3 the monocationic SbCl2+ complexes [SbCl2(L)]+ (L = mn-15S20 3, mn-18S20 4) were detected. NaSbCl6 and mn-18S20 4 in M eCN furnished the 2:1 complex [Na(mn-18S20 4)2]SbCl6 {(5)SbCl6). In the com plex cation 5 the sodium atom is coordinated sandwich-like through the eight oxygen atoms of two mn-18S20 4 molecules. Compound (5)SbCl6 crystallize in the triclinic space group P -1 with two formula units per unit cell. 
  Reference    Z. Naturforsch. 54b, 799 (1999); received September 24 1998 
  Published    1999 
  Keywords    Maleonitrile-Dithiacrown Ether Complexes, Antim ony and Bismuth Trichlorides, Sodium, Crystal Structure, D EP-M S 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0799.pdf 
 Identifier    ZNB-1999-54b-0799 
 Volume    54