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  • Analytical Chemistry and Spectroscopy  (48)
  • crystal structure  (6)
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 29 (1999), S. 513-521 
    ISSN: 1572-8854
    Keywords: nanotechnology ; molecular devices ; triptycene ; crown ether ; crystal structure ; thallium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The incorporation of 9,10-triptycene unit in a crown ether is examined from a structural perspective. Insertion of a triptycene group into 18-crown-6 stretches the crown into an ellipse, as seen in structures presented here of 9,10-triptyceno-22-crown-6 and its thallium complex. Symmetric addition of two triptycene groups into 18-crown-6 results in the sterically congested bis(9,10-triptyceno)-26-crown-6, whose crown cavity is filled with the π-clouds of two arene groups. The larger bis(9,10-triptyceno)-32-crown-8 is more sterically relaxed. The structures of these bis(triptyceno)crown ether molecules are the first with two triptycene groups simultaneously linked through their 9 and 10 positions, thereby forming a simple molecular gearing mechanism. The compound 9,10-triptyceno-22-crown-6 (1) crystallizes in the orthorhombic space group Pbca with a = 10.7962(7), b = 15.826(3), c = 31.147(5) Å, V = 5321.8(12) Å3, and Z = 8; its complex with TlNO3 (Tl-1) crystallizes in the monoclinic space group P21/c with a = 8.1884(14), b = 19.552(2), c = 20.575(4) Å, β = 97.062(8)°, V = 3269.2(9) Å3, and Z = 4; bis(9,10-triptyceno)-26-crown-6 (2) crystallizes in the triclinic space group P $$\bar 1$$ with a = 8.6488(11), b = 10.7718(12), c = 12.3324(12) Å, α = 111.58(1), β = 100.55(1), γ = 106.43(1)°, V = 970.3(5) Å3, and Z = 1; and bis(9,10-triptyceno)-32-crown-8 (3) crystallizes in the orthorhombic space group Pna21 with a = 20.186(3), b = 8.558(2), c = 25.623(2) Å, V = 4426.2(14) Å3, and Z = 4.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1572-8862
    Keywords: Rhenium ; dirhenium complexes ; rhenium-rhenium multiple bonds ; isocyanide ligands ; carbonyl ligand ; structural isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The monocarbonyl complex Re2Cl4(µ-dppm)2(CO) reacts with xylyl isocyanide in acetonitrile to afford the bioctahedral complex (CO)Cl2Re(µ-dppm)2 ReCl2(CNxyl), 2b. This is a different structural isomer from the edge-sharing bioctahedral complex Cl2Re(µ-Cl)(µ-dppm)2ReCl(CNxyl) or this same stoichiometry which A formed when acetone is be reaction solvent. The complex2b reacts with a further equivalent of xylNC in the presence of TlO3SCF3 in dichloromethane to form a red complex of composition [Re2Cl3(µ-dppm)2 (CO)(CNxyl)2]O3SCF3. 3, which has the open bioctahedral structure [(xylNC)2ClRe(µ-dppm)2ReCl2(CO)]O3SCF3. This is a third isomeric form of this dirhenium cation: the previously isolated green and yellow forms have edge-sharing bioctahedral structures. Crystal data for3 at 295 K: orthorhombic space group Pbca (No. 61) witha=22.654(5) Å,b=22.717(4) Å,c=27.324(4) A,V= 14061(7) Å3, andZ = 8. The structure was refined to R = 0.059 (R, = 0.134 ) for 14164 data. The Re-Re distance is 2.3833(8) Å.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of chemical crystallography 29 (1999), S. 1255-1259 
    ISSN: 1572-8854
    Keywords: crown ether ; crystal structure ; lariat ; sodium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract A dibenzo-14-crown-4 ether with a novel monooxyacetone sidearm is prepared and its structure with sodium perrhenate is determined. The structure crystallizes in P21/c with cell dimensions: a = 8.107(2) Å, b = 28.138(3) Å, c = 10.293(2) Å, and β = 104.173(9)°; giving a volume of 2276.6(7) Å3. This structure is compared to other sodium complexes of dibenzo-14-crown-4 lariat ethers and is found to be the only one with intramolecular bonding between the sidearm and the cation. Possible reasons for this observation are discussed.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1572-8854
    Keywords: Amines ; crystal structure ; pentacycloundecane-8,11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structures of three compounds formedvia nucleophilic attack of a heterocyclic secondary amine on PCU-8,11-dione, with the concomitant intramolecular attack of one keto oxygen on the carbon of the other ketone, are presented. In all three compounds, the bridging oxygen contains substantial p-character, and the bonds to the “attacking” nitrogen are significantly shorter than would be expected.
    Type of Medium: Electronic Resource
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  • 5
    ISSN: 1572-8862
    Keywords: Rhenium ; dirhenium complexes ; rhenium–rhenium multiple bonds ; isocyanide ligands ; carbonyl ligand ; structural isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of the unsymmetrical, coordinatively unsaturated dirhenium(II) complex [(XylNC)(OC)CIRe(μ-dppm)2ReCl2]O3SCF3 (dppm = Ph2PCH2PPh2) with one equivalent of XylNC in CH2Cl2 affords a fifth structural isomer of the [Re2Cl3(μ-dppm)2(CO)(CNXyl)2] + cation; this is believed to have a CO-bridged structure of the type [(XylNC)ClRe(μ-Cl)(μ-CO)(μ-dppm)2ReCl(CNXyl)]+. The latter complex reacts with a further equivalent of XylNC in the presence of Tl+ to form the [Re2Cl2(μ-dppm)2(CO)(CNXyl)3]2+ cation, which has been shown by IR spectroscopy, and by the X-ray crystallographic characterization of its neutral congener Re2Cl2(μ-dppm)2(CO)(CNXyl)3, to contain a very weak and unsymmetrical CO bridge.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1988), S. 193-204 
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method which involves the use of tandem mass spectrometry (MS/MS) for the identification of drug metabolites has been demonstrated with a triple quadrupole mass spectrometer. The method is based on the fact that metabolites usually retain various substructures of the original drug molecule. MS/MS is capable of rapidly identifying molecules with characteristic substructures without prior separation. It is shown that this method makes it possible to postulate possible drug metabolite structures rapidly and systematically without the use of standards. The MS/MS method, as it was applied to the identification of the metabolites of a new antiepileptic drug, zonisamide, is discussed. In this case it was possible to identify isomeric metabolites due to their differences in vaporization times off the probe and their different daughter spectra. The complementary uses of the neutral loss and parent scans for the determination of the site of metabolism is demonstrated. A new figure of merit, the limit of identification, is introduced. The amount of the epoxide metabolite of carbamazepine necessary for its reliable identification in urine was shown to be 0.4 ng/μl. The application of various techniques to confirm preliminary findings with this MS/MS method are described.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 26 (1996), S. 197-207 
    ISSN: 1573-1111
    Keywords: Crown ether ; nitromethane complex ; coordination isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray diffraction analyses of two nitromethane complexes of furanotribenzo-21-crown-7 (1 and2) and the nitromethane complex of dibenzo-2l-crown-7 (3) are reported. The two nitromethane complexes1 and2 are polymorphic in that the macrocyclic ring adopts the ‘dentist's chair’ conformation in both structures, with a single nitromethane molecule coordinating to either the lower, concave (1) or upper, convex (2) face of the crown ether. Complex3 adopts an entirely different conformation with a coplanar arrangement of the crown ether oxygen atoms binding a single nitromethane molecule.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 52-52 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 29-32 
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; electroosmotic flow ; frit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The formation of bubbles in capillary electrochromatography (CEC) is well documented: possible origins include Joule heating and variations in EOF velocity on passing from the stationary phase through the frit and into the open tube. Methods for the prevention of bubble formation are discussed which are confirmed by experimental results. Using frit lengths varying from 1 mm to 6 mm it is shown how frit length is directly related to the likelihood of bubble formation and how this is affected by applied voltage. It is shown that the change in applied voltage across a capillary affects the formation of bubbles and also that rebonding octadecylsilane (ODS) onto the silica frit after formation of the frit can minimize the formation of bubbles and how this effects the chromatography. A method is also described for increasing the robustness of silica capillaries using a column coupler along with modifications made to conventional capillary electrophoresis equipment to cater for CEC.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 478-479 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Kováts retention index ; GW-BASIC program ; Computer-assisted calculation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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