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1Author    BisacetonitrilRequires cookie*
 Title    Kristallstruktur von Hydrogenoxonium-Hexachloroantimonat  
 Abstract    The formation of hydrogen bonds to acetonitrile molecules lends stability to the hitherto un­ known hydrogenoxonium hexachloroantimonate H30 +SbCl6_ . The structure of H30 +SbCl6~ • 2 CH3CN was determined on a single crystal. It crystallises in the orthorhombic space group Pmn2(1) (Nr. 31) with Z = 2, a = 1 12,7(1),b = 988,8(1) and c = 1036,5(1) pm. 
  Reference    Z. Naturforsch. 54b, 377—380 (1999); eingegangen am 2. Dezember 1998 
  Published    1999 
  Keywords    Hydrogenoxonium Hexachloroantimonate Bisacetonitrile, Crystal Structure, Raman Data, Hydrogen Bonds 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0377.pdf 
 Identifier    ZNB-1999-54b-0377 
 Volume    54 
2Author    K. Dallmann, W. PreetzRequires cookie*
 Abstract    Normalkoordinatenanalyse von [Os(acac)3] Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis o f [Os(acac)3] In the reaction o f K 2[O sCl6] with boiling water/acetylacetone (1:1) a mixture o f different chloro-acetylacetonato complexes is formed, from which [Os(acac)3] can be isolated by column chromatography with dichloromethane on silica gel. The crystal structure o f [Os(acac)3] (m o­ noclinic, space group P2,/c,a = 13.968(5), b = l . 517(5), c = 16.455(5) A ,ß = 98.939(5)°, Z = 4) has been determined by single crystal X-ray diffraction analysis. High resolution IR and Raman spectra were measured at low temperature (10 K). Based on the molecular parameters o f the X-ray structure determination a normal coordinate analysis has been performed and the normal modes o f vibration have been assigned. With a set o f 32 force constants, taking into account the intraligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants are fd(OsO) = 3.19 and fd(O C) = 6.74 mdyn/A. 
  Reference    Z. Naturforsch. 53b, 232—238 (1998); eingegangen am 26. November 1997 
  Published    1998 
  Keywords    Tris(acetylacetonato)osmium(III), Crystal Structure, IR Data, Raman Data, Normal Coordinate Analysis 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0232.pdf 
 Identifier    ZNB-1998-53b-0232 
 Volume    53 
3Author    R. Nagel3, M. Botovab, G. Pracht3, E. Suchanek3, M. Manevab, H. D. Lutz3 ', HerrnRequires cookie*
 Title    Kristallstruktur, Infrarot-und Ramanspektren sowie thermische Zersetzung von Magnesiumtetrahydrogendimesoperiodat, MgH4I2O10 * 6H20 Crystal Structure, Infrared and Raman Spectra and Thermal Decomposition of Magnesium Tetrahydrogen Dimesoperiodate, MgH4I2O ,0 * 6H20  
 Abstract    Crystal structure, DRIFT, infrared and Raman spectra, and the results of thermal analyses of the hitherto wrongly as Mg(H4I 0 6)2 • 4H20 and M g(I04) • 8H20 described dimesoperiodate MgH4I2O l0 • 6H20 and of the isostructural zinc compound are presented. The compounds crystallize in the monoclinic space group P2, (Z = 2) with a = 1071.0(2), b = 547.0(1), c = 1194.9(2) pm, and ß = 112.58(3)° and a = 1073.3(3), b = 545.3(2), c = 1188.3(5) pm, and ß = 112.52(3)°, respectively. The structure, which was refined from X-ray single crystal data of the magnesium compound (R 1 = 2.72%, 3824 independet reflections}, is built up from isolated distorted M(H20) 62+ octahedra and dimesoperiodate ions H4I2O 10 -connected by a network of hydrogen bonds formed by the H4I2O 10"~ ions and six crystallographically different hydrate H20 molecules. The strength of the hydrogen bonds ranges from unusually weak bonds corresponding to uncoupled (isotopically dilute samples) OD stretching modes of > 2600 cm-1 and ver^ strong ones (uOD: < 2200 cm-1). The IO stretching modes of the trans-configurated H4I2O l0~-ions are assigned to terminal 1-0 groups (816 cm-1), I-OH groups (746 and 762 cm' 1) and bridging 1-0 groups (618 and 647 cm-1). On heating, MgH4I2O |0 • 6H20 undergoes dehydration in the range of 373 -485 K (Differential Scanning Calorimetry) to two different polymorphs of magnesium metaperiodate (H4I2O |02-—» ■ 2 I0 4-+ 2H20). Anhydrous M g(I04)2 is instable. Above 423 K (high-temperature Raman data), it decomposes to magnesium iodates. 
  Reference    Z. Naturforsch. 54b, 999—1008 (1999); eingegangen am 16. April 1999 
  Published    1999 
  Keywords    Magnesium Periodate Hydrate, Zinc Periodate Hydrate, Dimesoperiodate Ions, Crystal Structure, Raman Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0999.pdf 
 Identifier    ZNB-1999-54b-0999 
 Volume    54 
4Author    Jürgen Schatz3, Frank Schildbacha, AxelL.Requires cookie*
 Title    The Inclusion of Carbon Disulfide in /?-rerf-Butylcalix[4]-and [6 ]arene - A Combined Crystallographic and Vibrational Spectroscopic Study  
 Abstract    en tzb, Sylvia R a stä tte rb, Joachim Schilling5, Jö rg D o rm an n c, A n d reas R uoffc, and Tony D eb ae rd em ae k erd The inclusion complexes formed from carbon disulfide and /?-r£7-r-butylcalix[4]arene (1 C S 2) or /?-rm-butylcalix[6]arene (2-C S2) were investigated by X-ray crystal structure analysis, infrared (IR) and Raman spectroscopy. The complex 1 C S 2 crystallises in the space group P4/n, 2 C S 2 in the space group P2xln. In case of /?-rm-butylcalix[4]arene as host the carbon disulfide molecule is included in the cavity. In the crystal structure of p-rm -butylcali-x[6]arene clathrate, self-com plexation o f one rm-butyl group in the cavity o f another ca-lix[6]arene can be observed. Due to inclusion, the symmetry of CS2 is lowered both in the p-rm -butylcalix[4]arene and p-rm-butylcalix[6]arene case causing significant shifts in the fully assigned infrared and Raman spectra. 
  Reference    Z. Naturforsch. 55b, 213—221 (2000); received N ovem ber 16. 1999 
  Published    2000 
  Keywords    p-rerz-Butylcalixarenes, Inclusion Complexes, Crystal Structure, IR Data, Raman Data 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0213.pdf 
 Identifier    ZNB-2000-55b-0213 
 Volume    55