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  • 1
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    Crystal structure of ammonium/potassium trans-bis(N-methyliminodiacetato-κ3O,N,O′)chromate(III) from synchrotron data (2016)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2016-07-23
    Description: The structure of the title compound, [(NH4)0.8K0.2][Cr(C5H7NO4)2] (C5H7NO4 is methyliminodiacetate; mida), has been determined from synchrotron data. The CrIII atom is located on a centre of symmetry and is coordinated by two N atoms and four O atoms of two facially arranged tridentate mida ligands, displaying a slightly distorted octahedral coordination environment. The Cr—N and mean Cr—O bond lengths are 2.0792 (14) and 1.958 (14) Å, respectively. The cation site is located on a twofold rotation axis and shows occupational disorder, being occupied by ammonium and potassium cations in a 0.8:0.2 ratio. In the crystal, intermolecular hydrogen bonds involving the N—H groups of the ammonium cation as donor and the two non-coordinating O atoms of the carboxylate group as acceptor groups consolidate the three-dimensional packing.
    Keywords: crystal structuresynchrotron radiationammonium/potassium saltbis(methyliminodiacetato)chromate(III) ionmidatrans-facial configurationhydrogen bonding
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography (IUC)
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  • 2
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    Crystal structure of ammonium bis(pyridine-2,6-dicarboxylato-κ3O,N,O′)chromate(III) from synchrotron data (2015)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2015-01-25
    Description: The structure of the title compound, (NH4)[Cr(pydc)2] (pydc is pyridine-2,6-dicarboxylate, C7H3NO4), has been determined from synchrotron data. The CrIII ion and the N atom of the ammonium cation are located on a crystallographic fourfold rotoinversion axis (-4). The CrIII cation is coordinated by four O atoms and the two N atoms of two meridional pydc ligands, displaying a distorted octahedral geometry. The Cr—N and Cr—O bond lengths are 1.9727 (15) and 1.9889 (9) Å, respectively. The crystal structure is stabilized by intermolecular hydrogen bonds involving the N–H groups of the ammonium cation and pyridine C–H groups as donors and the non-coordinating carbonyl O atoms as acceptors.
    Keywords: Crystal structuresynchrotron radiationpyridine-2,6-dicarboxylateammonium cationchromate(III) complexmeridional configurationhydrogen bonding
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography (IUC)
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  • 3
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    Crystal structure of tris(trans-1,2-cyclohexanediamine-κ2N,N′)chromium(III) tetrachloridozincate chloride trihydrate from synchrotron data (2016)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2016-04-13
    Description: The structure of the title double salt, [Cr(rac-chxn)3][ZnCl4]Cl·3H2O (chxn is trans-1,2-cyclohexanediamine; C6H14N2), has been determined from synchrotron data. The CrIII ion is coordinated by six N atoms of three chelating chxn ligands, displaying a slightly distorted octahedral coordination environment. The distorted tetrahedral [ZnCl4]2− anion, the isolated Cl− anion and three lattice water molecules remain outside the coordination sphere. The Cr—N(chxn) bond lengths are in a narrow range between 2.0737 (12) and 2.0928 (12) Å; the mean N—Cr—N bite angle is 82.1 (4)°. The crystal packing is stabilized by hydrogen-bonding interactions between the amino groups of the chxn ligands and the water molecules as donor groups, and O atoms of the water molecules, chloride anions and Cl atoms of the [ZnCl4]2− anions as acceptor groups, leading to the formation of a three-dimensional network. The [ZnCl4]2− anion is disordered over two sets of sites with an occupancy ratio of 0.94:0.06.
    Keywords: crystal structure1,2-cyclohexanediaminetetrachloridozincate chloride double saltchromium(III) complexhydrogen bondingsynchrotron radiation
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography (IUC)
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  • 4
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    Crystal structure of trans-bis(ethane-1,2-diamine-κ2N,N′)bis(thiocyanato-κN)chromium(III) perchlorate from synchrotron data (2015)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2015-05-21
    Description: The structure of the title compound, [Cr(NCS)2(C2H8N2)2]ClO4, has been determined from synchroton data. The asymmetric unit consists of one half of a centrosymmetric CrIII complex cation and half of a perchlorate anion with the Cl atom on a twofold rotation axis. The CrIII ion is coordinated by the four N atoms of two ethane-1,2-diamine (en) ligands in the equatorial plane and two N-bound thiocyanate (NCS−) anions in a trans-axial arrangement, displaying a slightly distorted octahedral geometry with crystallographic inversion symmetry. The Cr—N(en) bond lengths are in the range 2.053 (16)–2.09 (2) Å, while the Cr—N(thiocyanate) bond length is 1.983 (2) Å. The five-membered en rings are disordered over two sites, with occupancy ratios of 0.522 (16):0.478 (16). Each ClO4− anion is disordered over two sites with equal occupancy. The crystal structure is stabilized by intermolecular hydrogen bonds involving the en NH2 groups as donors and perchlorate O and thiocyanate S atoms as acceptors.
    Keywords: crystal structuresynchrotron radiationethane-1,2-diaminethiocyanatetrans-geometrychromium(III) complexhydrogen bonds
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
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  • 5
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    Crystal structure of trans-dichlorido(1,4,8,11-tetraazaundecane-κ4N)chromium(III) perchlorate determined from synchrotron data (2016)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2016-02-25
    Description: The structure of the title complex, [CrCl2(2,3,2-tet)]ClO4 (2,3,2-tet is 1,4,8,11-tetraazaundecane, C7H20N4), has been determined from synchrotron data. The CrIII ion is coordinated by the four N atoms of the 1,4,8,11-tetraazaundecane ligand in the equatorial plane and two chloride ions in an axial arrangement, displaying a slightly distorted octahedral coordination environment. The two H atoms of the secondary amines are grouped on the same side of the equatorial N4 plane (meso-RS conformation). The Cr—N bond lengths range from 2.069 (2) to 2.084 (2) Å, while the mean Cr—Cl bond length is 2.325 (2) Å. The crystal structure is stabilized by intermolecular hydrogen-bonding interactions between the primary and secondary amine groups of the 2,3,2-tet ligands, the Cl ligands and the O atoms of the perchlorate counter-anion, forming corrugated layers parallel to (010).
    Keywords: crystal structure1,4,8,11-tetraazaundecanechloride ligandtrans–meso (RS) conformationchromium(III) complexhydrogen bondingsynchrotron radiation
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography (IUC)
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  • 6
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    Crystal structure of trans-difluoridotetrakis(pyridine-κN)chromium(III) trichlorido(pyridine-κN)zincate monohydrate from synchrotron data (2014)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2014-10-05
    Description: In the asymmetric unit of the title compound, [CrF2(C5H5N)4][ZnCl3(C5H5N)]·H2O, there are two independent complex cations, one trichlorido(pyridine-κN)zincate anion and one solvent water molecule. The cations lie on inversion centers. The CrIII ions are coordinated by four pyridine (py) N atoms in the equatorial plane and two F atoms in a trans axial arrangement, displaying a slightly distorted octahedral geometry. The Cr—N(py) bond lengths are in the range 2.0873 (14) to 2.0926 (17) Å while the Cr—F bond lengths are 1.8609 (10) and 1.8645 (10) Å. The [ZnCl3(C5H5N)]− anion has a distorted tetrahedral geometry. The Cl atoms of the anion were refined as disordered over two sets of sites in a 0.631 (9):0.369 (9) ratio. In the crystal, two anions and two water molecules are linked via O—H...Cl hydrogen bonds, forming centrosymmetric aggregates. In addition, weak C—H...Cl, C—H...π and π–π stacking interactions [centroid–centroid distances = 3.712 (2) and 3.780 (2)Å] link the components of the structure into a three-dimensional network.
    Keywords: crystal structurefluoride ligandpyridine ligandtrans-isomerchromium(III) complex
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
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  • 7
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    Crystal structure of trans-diammine(1,4,8,11-tetraazacyclotetradecane-κ4N)chromium(III) tetrachloridozincate chloride monohydrate from synchrotron data (2016)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2016-03-05
    Description: The asymmetric unit of the title complex salt, [Cr(C10H24N4)(NH3)2][ZnCl4]Cl·H2O, is comprised of four halves of the CrIII complex cations (the counterparts being generated by application of inversion symmetry), two tetrachloridozincate anions, two chloride anions and two water molecules. Each CrIII ion is coordinated by the four N atoms of the cyclam (1,4,8,11-tetraazacyclotetradecane) ligand in the equatorial plane and by two N atoms of ammine ligands in axial positions, displaying an overall distorted octahedral coordination environment. The Cr—N(cyclam) bond lengths range from 2.0501 (15) to 2.0615 (15) Å, while the Cr—(NH3) bond lengths range from 2.0976 (13) to 2.1062 (13) Å. The macrocyclic cyclam moieties adopt the trans-III conformation with six- and five-membered chelate rings in chair and gauche conformations. The [ZnCl4]2− anions have a slightly distorted tetrahedral shape. In the crystal, the Cl− anions link the complex cations, as well as the solvent water molecules, through N—H...Cl and O—H...Cl hydrogen-bonding interactions. The supramolecular set-up also includes N—H...Cl, C—H...Cl, N—H...O and O—H...Cl hydrogen bonding between N—H or C—H groups of cyclam, ammine N—H and water O—H donor groups, and O atoms of the water molecules, Cl− anions or Cl atoms of the [ZnCl4]2− anions as acceptors, leading to a three-dimensional network structure.
    Keywords: crystal structurecyclamammine ligandtetrachloridozincate chloride double salttrans-III conformationchromium(III) complex
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
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  • 8
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    Crystal structure of trans-cyclohexane-1,2-diammonium chromate(VI) from synchrotron X-ray diffraction data (2016)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2016-12-06
    Description: The structure of the title hybrid compound, (C6H16N2)[CrO4], has been determined from synchrotron data. The organic cation adopts a chair conformation. The inorganic CrO42− anion is slightly distorted owing to its involvement in N—H...O hydrogen-bonding interactions with neighbouring trans-cyclohexane-1,2-diammonium cations, whereby the two Cr—O bonds to the O atoms acting as acceptor atoms for two hydrogen bonds are slightly longer than the other two Cr—O bonds for which only one acceptor interaction per O atom is observed. In the crystal, cations and anions are packed into layers parallel to (001), held together through the aforementioned N—H...O hydrogen bonds.
    Keywords: crystal structuretrans-cyclohexane-1,2-diammoniumchromate(VI)hydrogen bondingsynchrotron radiationhybrid compound
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
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  • 9
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    Crystal structure of bis[(oxalato-κ2O1,O2)(1,4,8,11-tetraazacyclotetradecane-κ4N)chromium(III)] dichromate octahydrate from synchrotron X-ray data (2017)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2017-02-17
    Description: The asymmetric unit of the title compound, [Cr(C2O4)(C10H24N4)]2[Cr2O7]·8H2O (C10H24N4 = 1,4,8,11-tetraazacyclotetradecane, cyclam; C2O4 = oxalate, ox) contains one [Cr(ox)(cyclam)]+ cation, one half of a dichromate anion that lies about an inversion centre so that the bridging O atom is equally disordered over two positions, and four water molecules. The terminal O atoms of the dichromate anion are also disordered over two positions with a refined occupancy ratio 0.586 (6):0.414 (6). The CrIII ion is coordinated by the four N atoms of the cyclam ligand and one bidentate oxalato ligand in a cis arrangement, resulting in a distorted octahedral geometry. The Cr—N(cyclam) bond lengths are in the range 2.069 (2)–2.086 (2) Å, while the average Cr—O(ox) bond length is 1.936 Å. The macrocyclic cyclam moiety adopts the cis-V conformation. The dichromate anion has a staggered conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups and water O—H groups as donors, and the O atoms of oxalate ligand, water molecules and the Cr2O72− anion as acceptors, giving rise to a three-dimensional network.
    Keywords: crystal structurecyclamchromium(III) complexbidentate oxalato ligandcis-V conformationdichromate anionhydrogen bondingsynchrotron radiation
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
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  • 10
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    Crystal structure of [2,13-bis(acetamido)-5,16-dimethyl-2,6,13,17-tetraazatricyclo[16.4.0.07,12]docosane-κ4N]silver(II) dinitrate from synchrotron X-ray data (2018)
    International Union of Crystallography (IUC)
    Details
    Publication Date: 2018-03-06
    Description: The asymmetric unit of the title compound, [Ag(C24H46N6O2)](NO3)2 [C24H46N6O2 is (5,16-dimethyl-2,6,13,17-tetraazatricyclo[16.4.0.07,12]docosane-2,13-diyl)diacetamide, L], consists of one independent half of the [Ag(C24H46N6O2)]2+ cation and one nitrate anion. The Ag atom, lying on an inversion centre, has a square-planar geometry and the complex adopts a stable trans-III conformation. Interestingly, the two O atoms of the pendant acetamide groups are not coordinated to the AgII ion. The longer distance of 2.227 (2) Å for Ag—N(tertiary) compared to 2.134 (2) Å for Ag—N(secondary) may be due to the effects of the attached acetamide group on the tertiary N atom. Two nitrate anions are very weakly bound to the AgII ion in the axial sites and are further connected to the ligand of the cation by N—H...O hydrogen bonds. The crystal packing is stabilized by hydrogen-bonding interactions among the N—H donor groups of the macrocycle and its actetamide substituents, and the O atoms of the nitrate anions and of an acetamide group as the acceptor atoms.
    Keywords: crystal structuremacrocyclesynchrotron radiationsilver(II) complex nitrate iontrans-III conformationhydrogen bonding
    Electronic ISSN: 1600-5368
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography (IUC)
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