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  • 1
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 55 (1999), S. 104-113 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The dipeptide L-Leu-L-Val can crystallize as a hydrate in the hexagonal space group P65 [Görbitz & Gundersen (1996). Acta Chem. Scand. 50, 537–543], but forms 1:1 solvates when methanol, ethanol and 2-propanol are used as precipitating agents. The structures of these complexes can be divided into hydrophobic and hydrophilic layers. The alcohol molecules are embedded in the hydrophobic layers, but with the hydroxyl groups as crucial parts of the hydrogen-bonding network. L-Leucyl-L-valine–methanol (1/1) crystallizes in the space group P21 with Z = 2. L-Leucyl-L-valine–ethanol (1/1) has very special systematic absences, and the structure could not be solved with direct methods. Unraveling the actual build-up of the crystal was an unusual process involving modeling with molecular graphics programs. The solution shows a structure which formally belongs to the space group P21, with four dipeptide molecules and four solvent molecules in the asymmetric unit (Z = 8). Additional non-crystallographic symmetry in three dimensions fixes all cell angles, including β, to 90°. L-Leucyl-L-valine–2-propanol (1/1) is structurally closely related to the ethanol solvate, but owing to a rare type of packing disorder the length of the a axis is halved (Z = 4, P212121). The hydrogen-bonding pattern is still the same as in the ethanol solvate, which means that the hydrogen-bond periodicity along the a axis in the 2-propanol solvate is two unit-cell lengths.
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  • 2
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. 715-719 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: DL-Allylglycine (DL-2-amino-4-pentenoic acid, C5H9NO2) yields crystals with Pca21 symmetry and two crystallographically independent yet pseudo-inversion-related enantiomers. The distribution among the common space groups of other crystalline racemates with more than one molecule in the asymmetric unit has been established. The conformational similarities between crystallographically independent enantiomers in 114 non-centrosymmetric racemates were quantified using the r.m.s. deviation for a molecular superposition. The analysis shows that in the majority of crystals the conformations of the crystallographically independent molecules are very similar with mean r.m.s. deviation = 0.190 Å. In almost 80% of the structures the mean r.m.s. deviations is in the interval 0–0.2 Å. It is estimated that racemates constitute 23% of the centrosymmetric organic structures in the Cambridge Structural Database.
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  • 3
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. 1094-1102 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Useful information about hydrogen bonding, the preferred modes of hydrophobic interaction and conformational preferences of a specific molecule can be obtained from cocrystallization of the solute with a selected series of solvent molecules. This method is used in a study of nine different crystal structures of diethylstilbestrol (DES) solvates. It is shown that solvent inclusion results not only in stronger hydrogen bonds, but usually also in a larger number of favorable C—H...π interactions between DES molecules. Furthermore, solvent molecules such as DMSO, DMF, acetonitrile and acetone demonstrate important hydrogen-bond donating properties in addition to their more familiar role as hydrogen-bond acceptors. Molecular conformations in the crystal structures compare favorably with results from molecular mechanics calculations.
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  • 4
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. 526-534 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The Cambridge Structural Database has been searched for all crystal structures including organic solvent molecules (solvates) and solvent water molecules (hydrates). Well above 300 different solvent molecules were identified and the frequencies with which they occur in crystal structures, as a function of the year of publication, were established. The crystal structures are classified as `organic' and `metalloorganic'; it is shown that the relative prevalences of various cocrystallized solvents are different in the two groups. Several frequently used organic solvents are also common ligands for metal ions. Special interest has been focused on the existence of heterosolvates, i.e. crystal structures which include more than one type of solvent molecule. Up to five different types of solvent molecules were found in a single crystal structure. It is suggested that the use of solvent mixtures during crystallizations may prove to be a more useful and versatile approach for obtaining crystals of high-molecular-weight organic compounds than has hitherto been recognized.
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  • 5
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. e23-e24 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The structure of taurine (2-aminoethanesulfonic acid), C2H7NO3S, has been redetermined at 150 K, and is compared with the structures of glycine and β-alanine which, like taurine, are enzymatically conjugated with bile acids.
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  • 6
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. e64-e65 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The crystal structure of the title compound, C8H16N2O3S·2C3H8O, is divided into hydrophobic and hydrophilic layers. Two peptide molecules in the asymmetric unit are related by pseudo-translational symmetry along the a axis, as are two of the four 2-propanol molecules. The last two 2-propanol molecules in the asymmetric unit have different relative orientations and hydrogen-bond interactions.
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  • 7
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 57 (2001), S. 575-576 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: A new type of molecular arrangement for dipeptides is observed in the crystal structure of L-phenylalanyl-L-alanine dihydrate, C12H16N2O3·2H2O. Two L-Phe and two L-Ala side chains aggregate into large hydrophobic columns within a three-dimensional hydrogen-bond network.
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  • 8
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 57 (2001), S. o192-o194 
    ISSN: 1600-5368
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The asymmetric unit of the title compound, L-phenylalaninium nitrate tris(L-phenylalanine), C9H12NO2+·NO3−·3C9H11NO2, contains a nitrate anion and a peculiar sequence of four L-phenylalanine molecules. Three of them are present as zwitterions, while the last carries the positive charge and acts as donor in a –COOH...−OOC– hydrogen bond with an O...O distance of 2.443 (9) Å.
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  • 9
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 55 (1999), S. 424-431 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The amino acid L-isoleucine has been cocrystallized with seven selected D-amino acids including D-methionine [L-isoleucine–D-methionine (1/1), C6H13NO2.C5H11NO2S, amino-acid side chain R = —CH2—CH2—S—CH3] and a homologous series from D-alanine [L-isoleucine–D-alanine (1/1), C6H13NO2.C3H7NO2, R = —CH3] through D-α-aminobutyric acid [L-isoleucine–D-α-aminobutyric acid (1/1), C6H13NO2.C4H9NO2, R = —CH2—CH3] and D-norvaline [L-isoleucine–D-norvaline (1/1), C6H13NO2.C5H11NO2, R = —CH2—CH2—CH3] to D-norleucine [L-isoleucine–D-norleucine (1/1), C6H13NO2.C6H13NO2, R = —CH2—CH2—CH2—CH3] with linear side chains, and D-valine [L-isoleucine–D-valine (1/1), C6H13NO2.C5H11NO2, R = —CH—(CH3)2] and D-leucine [L-isoleucine–D-leucine (1/1), C6H13NO2.C6H13NO2, R = —CH2—CH—(CH3)2] with branched side chains. All the crystal structures are divided into distinct hydrophilic and hydrophobic layers. In the five complexes with amino acids with linear side chains the polar parts of the D- and L-amino acids are related by pseudo-glide-plane symmetry, and four of them have remarkably similar molecular arrangements. The D-valine and D-leucine complexes, on the other hand, are structurally quite different with the polar parts of the D- and L-amino acids related by pseudo-inversion. Differences in the hydrogen-bond pattern in the two molecular arrangements are discussed.
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  • 10
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 55 (1999), S. 1090-1098 
    ISSN: 1600-5740
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The dipeptide Gly-L-Ser was crystallized as part of a study on hydrogen-bonding patterns in the structures of dipeptides. Hydrogen-bond donors and acceptors have been assigned ranks (1 is best, 2 is next best etc.), and the observed hydrogen-bond connectivity is compared with the hypothetical pattern in which the rank n donor associates with the rank n acceptor (n = 1, 2, . . .), and with the pattern observed in the retroanalogue L-Ser-Gly, which contains the same functional groups. Crystallization of the title compound produced very bulky crystals. Rather than reducing the size of one of these before data collection, three data sets with different exposure times were collected with a Siemens SMART CCD diffractometer on a very large specimen (2.2 × 2.0 × 0.8 mm). The crystal was subsequently shaped into a 0.30 mm-diameter sphere for collection of two additional data sets. The discussion of the refinement results focus on the effect of absorption correction for the various data sets, and a comparison of geometrical and thermal parameters. One advantage of using a large crystal, the great speed with which data can be obtained, has been exemplified by collection of a complete data set of good quality in less than 25 min.
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