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2000 (2)
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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    VladimirA. Ovchynnikov3, VladimirM. Amirkhanov3 ', TarasP. Timoshenko3, Tadeusz Glowiakb, Henryk KozlowskibRequires cookie*
 Title    Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide  
 Abstract    Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(0)NHP(0)[N(CH2CH2)2 0 ] 2 [HL] and its sodium [NaL] and morpholine [HN(CH2CH2) 2 0 HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) A, b = 16.056(3) A, c = 9.622(2) Ä, ß = 108.55(3)°, space group P2i/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups. 
  Reference    Z. Naturforsch. 53b, 481—484 (1998); received November 11 1997 
  Published    1998 
  Keywords    Carbacylamidophosphates, IR Data, X-Ray Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0481.pdf 
 Identifier    ZNB-1998-53b-0481 
 Volume    53 
3Author    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 
4Author    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 
5Author    S. I. El-Desokya, E. M. Kandeel3, A. H. Abd El-Rahm, R. R. Ana, ShmidtbRequires cookie*
 Title    Synthesis of Pyrrolo-, Thienopyrrolo-, Benzothienopyrroloquinolines as well as Triazoloindole Derivatives  
 Abstract    Substituted pyrroloquinoline, thienopyrroloquinoline, benzothieno-pyrroloquinoline and triazoloindole derivatives have been synthesized starting from 6-amino-2,3-diphenylindole. The structures of the newly synthesized compounds and MS data. 
  Reference    Z. Naturforsch. 53b, 1216—1222 (1998); received May 4 1998 
  Published    1998 
  Keywords    Pyrroloquinoline, Triazoloindole Derivatives, NM R Data, IR Data, MS Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1216.pdf 
 Identifier    ZNB-1998-53b-1216 
 Volume    53 
6Author    Christoph Mockenhaupt, Ralf Eßmanna, HeinzDieter LutzRequires cookie*
 Title    [Ni(NH3 )6]S0 4 : Kristallstruktur und Infrarotspektren [Ni(NH3)6]S 0 4: Crystal Structure and Infrared Spectra  
 Abstract    The crystal structure of [Ni(NH3)6]S 0 4 has been determined by single-crystal X-ray dif­ fraction (P2,/c; Z = 4; a = 705.0(1), b = 1195.2(2), c = 1180.0(2) pm, ß = 96.14(3)°; 2271 reflections; R x = 3.94%). In the hitherto unknown structure type, both the [Ni(NH3)6]2+ and the S 0 42-ions form chains along [100], The six crystallographically different ammine ligands of the distorted [Ni(NH3)6]2+ octahedra are involved in hydrogen bonds to six crystallographically equivalent S 0 42-ions (site symmetry C |). The strength of the hydrogen bonds differs strongly (i'od ° f matrix isolated N H 2D molecules: 2378 -2494 cm -1 , N -O distances: 272 -340 pm). The temperature evolution of the IR bands reveals the decrease of the dynamic orientational disorder of the N H 3 molecules with decreasing temperature. 
  Reference    Z. Naturforsch. 54b, 843—848 (1999); eingegangen am 8. März 1999 
  Published    1999 
  Keywords    Hexammine Nickel Sulfate, Ammoniates, Crystal Structure, IR Data, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0843.pdf 
 Identifier    ZNB-1999-54b-0843 
 Volume    54 
7Author    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 
8Author    K. Dallmann, W. PreetzRequires cookie*
 Title      
 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 
9Author    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