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  • 1
    Electronic Resource
    Electronic Resource
    Synthese von 6,7,8,9,15,16,17,18-Octahydrodibenzo[f,m][1,8,4,11]- dithiadiazacyclotetradecin-8,17-diessigsäure (H2L1); Strukturen entsprechender Kupfer-Komplexe (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1357-1362 
    Details
    ISSN: 0009-2940
    Keywords: Copper complexes ; Macrocyclic ligands, N-functionalized ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: trans-N2S2-Macrocyclic Ligands with Pendant Carboxylic Groups. - Synthesis of 6,7,8,9,15,16,17,18-Octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclotetradecine-8,17-diacetic Acid (H2L1); Structures of Corresponding Copper ComplexesThe macrocyclic ligand with pendant carboxylic groups 6,7,8,9,15,16,17,18-octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclotetradecine-8,17-diacetic acid (H2L1) and its Ni(II) and Cu(II) complexes, [NiL1]3(H3O·ClO4)4·H2O (1) and [Cu(HL1)]ClO4·1.5 H2O (2), have been prepared. The coordination properties of H2L1 towards Ni(II) and Cu(II) in aqueous solutions are independent on the pH according to UV/Vis-spectral measurements. The structures of 2 and of [CuL2]ClO4 (3) with HL2 = 6,7,8,9,15,16,17,18-octahydrodibenzo[f,m][1,8,4,11]dithiadiazacyclodetradecine-8-acetic acid have been determined by X-ray crystallography. In 2, all six donor atoms of the ligand are coordinated, forming an octahedron. Due to their size the metal atoms are not incorporated in the ligand cavity. The ligand is folded in such a way, that the N-donor atoms are in trans, and the S-(and O-)donor atoms in cis positions. In 3, the five donor atoms form a rather regular bipyramid with the N atoms in the axial positions. The stereochemistry of the ligands in the complexes 2 and 3 is discussed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19911240608
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and Crystal Structures of Copper(I) and Gold(I) Complexes [C(NH2)3]2[M2(1,2-dithiosquarate)2], M = Cu, Au, Containing Short M···M Distances, and of the Gold(III) Complex (cycloPrPh3P)[Au(1,2-dithiosquarate)2] (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 605-609 
    Details
    ISSN: 0009-2940
    Keywords: Copper(I) complexes ; Gold(I) complexes ; Dithiosquarates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new compounds [C(NH2)3]2[Cu2(dtsq)2] (1), [C(NH2)3]2-[Au2(dtsq)2] · H2O (2), and (cycloPrPh3P)[Au(dtsq)2] (3, cycloPr = cyclopropyl) have been prepared from CuSO4 · 5 H2O, KAuCl4, and K2dtsq · H2O (dtsq = dianion of 1,2-dithiosquaric acid, C4O2S2-2). Compounds 1 and 2 contain pairs of metal atoms with short intermetallic distances of 2.587(2) (Cu···Cu) and 2.846(2) Å (Au···Au). Cu(I) is trigonally coordinated to three sulfur atoms of three different ligands and lies 0.51 Å above the S3 plane. It is oriented towards the copper atom of a second CuS3 unit related to the first one by a center of inversion. Au(I) shows a linear coordination, leading to the formation of Au2(dtsq)2-2 dimers. These have intermolecular Au···Au distances of 3.259(2) Å. Compound 3 contains isolated Au(dtsq)-2 ions with square planar coordination geometry stacked along the a axis at 4.708 Å distance.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941270404
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  • 3
    Electronic Resource
    Electronic Resource
    Pyrrolo[1,2-b]cinnolin-6,8-dicarbonsäure-diethylester: Produkt einer anomalen Vilsmeier-Reaktion (1990)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1990 (1990), S. 627-630 
    Details
    ISSN: 0170-2041
    Keywords: Vilsmeier reaction, anomalous ; Pyrrolo[1,2-b]cinnoline, derivative ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diethyl Pyrrolo[1,2-b]cinnoline-6,8-dicarboxylate, a Product of an Anomalous Vilsmeier ReactionA byproduct of the Vilsmeier reaction of 1 has been shown by X-ray structure determination to be the pyrrolo[1,2-b]cinnoline 3. Informations concerning the mechanism of formation of 3 have been obtained from labeling experiments and an unequivocal assignment of NMR spectra.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.1990199001120
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  • 4
    Electronic Resource
    Electronic Resource
    Synthese und Struktur der Cobalt(III)-Komplexe 14gliedriger cis- und trans-N2S2-Dibenzomakrocyclen mit zwei koordinierenden AcetatogruppenProfessor Wolfgang Sawodny zum 60. Geburtstage gewidmet (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 796-800 
    Details
    ISSN: 0044-2313
    Keywords: Cobalt(III) complexes functionalized N2S2-macrocyclic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Cobalt(III) Complexes of 14-Membered cis- and trans-N2S2 Dibenzo Macrocycles with two Pendant Acetato GroupsThe isomeric fourteen membered macrocyclic ligands 6,7,9,15,16,18-hexahydrodibenzo[f,m][1,8]dithia[4,11]diazacyclotetradecine-8,17-diacetic acid-0.5-hydrate (H2L3), C22H26N2O4S2 · 0.5 H2O and 6,7,13,15,16,18-hexahydrodibenzo-[e,m][1,4]dithia[8,11]diazacyclotetradecine-14,17-diacetic acid-1.5-hydrate (H2L6), C22H26N2O4S2 · 1.5 H2O with cis- and trans-N2S2 donorsets and two pendant acetato groups form the stable complexes [Co(L3)]ClO4 · 2 H2O (1) and [Co(L6)]ClO4 · H2O (2). Co(III) is octahedrally coordinated herein to all six donor centers of the respective ligand. The macrocyclic rings are folded. The metal ions are located outside the macrocyclic cavity. The mean Co—N, Co—O and Co—S distances are 196, 190 and 224 pm, respectively.Crystal data: 1, monoclinic, space group C2/c, a = 3 797.7(9), b = 763.8(3), c = 2 207.0(7) pm, β = 123.17(2), Z = 8, 3 445 reflections, R(Rw) = 0.072(0.070); 2, monoclinic, space group C2/c, a = 3 197.1(6), b = 880.4(2), c = 1 890.6(4) pm, β = 112,19(3)°, Z = 8, 4 415 reflections, R(Rw) = 0.062(0.064).
    Notes: Die beiden isomeren Liganden 6,7,9,15,16,18-Hexahydrodibenzo[f,m][1,8]dithia[4,11]diazacyclotetradecin-8,17-diessigsäure-0,5-hydrat (H2L3), C22H26N2O4S2 · 0,5 H2O bzw. 6,7,13,15,16,18-Hexahydrodibenzo[e,m][1,4]dithia-[8,11]diazacyclotetradecin-14,17-diessigsäure-1,5-hydrat (H2L6), C22H26N2O4S2 · 1,5 H2O mit cis- bzw. trans-N2S2-Donorzentren im vierzehngliedrigen makrocyclischen Ring und zwei Acetat-Seitenketten bilden die stabilen Komplexe [Co(L3)]ClO4 · 2H2O (1) und [Co(L6)]ClO4 · H2O (2). CoIII ist jeweils von allen 6 Donorzentren der Liganden oktaedrisch umgeben. Die Liganden sind gefaltet. Die Metallatome liegen außerhalb der makrocyclischen Kavität.Kristalldaten: 1, monoklin, Raumgruppe C2/c, a = 3 797,7(9), b = 763,8(3), c = 2 207,0(7) pm, β = 123,17(2)°, Z = 8, 3 445 Reflexe, R(Rw) = 0,072(0,070); 2, monoklin, Raumgruppe C2/c, a = 3 197,1(6), b = 880,4(2), c = 1 890,6(4) pm, β = 112,19(3)°, Z = 8, 4415 Reflexe, R(Rw) = 0,062(0,064).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200506
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  • 5
    Electronic Resource
    Electronic Resource
    Nickel-, Palladium- und Platinkomplexe funktionalisierter Makrocyclen. Die Kristallstrukturen von [Ni(py2-tasn)(H2O)](ClO4)2, [Pd(py2-tasn)](PF6)2 und [Pt(py2-tasn)](PF6)2. (py2-tasn=4,7-Bis(2-methylpyridyl)-1-thia-4,7-diazacyclononanProfessor Harald Schäfer zum 80. Geburtstage gewidmet (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 158-162 
    Details
    ISSN: 0044-2313
    Keywords: Complexes of functionalized [9]-aneN2S ; Crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of [Ni(py2-tasn)(H2O)](ClO4)2, [Pd(py2-tasn)](PF6)2, and [Pt(py2-tasn)](PF6)2. (py2-tasn=4,7-Bis(2-methylpyridyl)-1-thia-4,7-diazacyclononane).The methylpyridyl functionalized macrocyclic ligand 4,7-Bis(2-methylpyridyl)-1-thia-4,7-diazacyclononane, py2-tasn, forms the stable complexes [Ni(py2-tasn)(H2O)]2+, [Pd(py2-tasn)]2+, and [Pt(py2-tasn)]2+. They have been isolated in the solid state and characterized by X-ray crystal structure analyses. All five donor atoms of the ligand are bound to the respective metal atom. NiII is octahedrally coordinated, with the pyridyl groups in cis-positions, PdII and PtII are square pyramidally coordinated, with the thioether group in the apical position. The Pd (Pt) - S distances are 290.7(1) and 305.6(3) pm, respectively.Crystal data: [Ni(py2-tasn)(H2O)](ClO4)4, orthorhombic, space group P212121, a=843.8(2), b=1 668.8(3), c=1 694.4(3) pm, Z=4, 2 444 unique data, R(Rw)=0.0825(0.0937); [Pd(py2-tasn)](PF6)2: monoclinic, space group P21/c, a=694.7(1), b=1 906.5(4), c=1 980.9(4) pm, β=93,43°, Z=4, 5 429 unique data, R(Rw)=0.0351(0.0451); [Pt(py2-tasn)](PF6)2: monoclinic, space group P21/n, a=1 080.1(2), b=1 175.0(2), c=2 075.6(4) pm, β=95.32(3)°, Z=4, 5 567 unique data, R(Rw)=0.0667(0.0845).
    Notes: Der methylpyridyl-funktionalisierte Ligand 4,7-Bis(2-methylpyridyl)-1-thia-4,7-diazacyclononan, py2-tasn, bildet die stabilen Komplexe [Ni(py2-tasn)(H2O)]2+, [Pd(py2-tasn)]2+ und [Pt(py2-tasn)]2+. Die Komplexe wurden als ClO4-- bzw. PF6--Salze isoliert und strukturell charakterisiert. Alle 5 Donorzentren des Liganden sind an die Zentralatome gebunden. NiII ist verzerrt oktaedrisch, mit den Pyridylgruppen in cis-Stellung, PdII und PtII quadratisch-pyramidal, mit der Thioether-Gruppe als apikalem Liganden koordiniert. Der Pd - S- bzw. Pt - S-Abstand beträgt 290,7(1) bzw. 305,6(3) pm.[Ni(py2-tasn)(H2O)]ClO4)4, orthorhombisch, Raumgruppe P212121 a=843,8(2), b=1 668,8(3), c=1 694,4(3) pm, Z=4, 2 444 unabhängige Reflexe, R(Rw)=0,082(0,094); [Pd(py2-tasn)](PF6)2: monoklin, Raumgruppe P21/c, a=694,7(1), b=1 906,5(4), c=1 980,9(4) pm, β=93,43°, Z=4, 5 429 unabhängige Reflexe, R(Rw)=0,035(0,045); [Pt(py2-tasn)](PF6)2: monoklin, Raumgruppe P21/n, a=1 080,1(2), b=1 175,0(2), c=2 075,6(4) pm, β=95,32(3)°, Z=4, 5 567 unabhängige Reflexe, R(Rw)=0,067(0,084).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936190126
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  • 6
    Electronic Resource
    Electronic Resource
    Darstellung, Ramanspektren und Kristallstrukturen von V2O3(SO4)2, K[VO(SO4)2] und NH4[VO(SO4)2]Herrn Professor Josef Grobe zum 60. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 158-164 
    Details
    ISSN: 0044-2313
    Keywords: Oxo-sulfato-vanadates(V) ; syntheses ; crystal structures ; Raman spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Raman Spectra, and Crystal Structures of V2O3(SO4)2, K[VO(SO4)2], and NH4[VO(SO4)2]The oxo-sulfato-vanadates(V) V2O3(SO4)2, K[VO(SO4)2], and NH4[VO(SO4)2] have been prepared as crystals suitable for X-ray structure determination. In all structures sulfate acts as an unidentate ligand only toward a single vanadium atom. The structure of V2O3(SO4)2 consists of a threedimensional network of pairs of cornershared VO6 octahedra with one terminal oxygen atom each, and SO4 tetrahedra. All oxygen atoms of the sulfate ions are coordinated. NH4[VO(SO4)2] and K[VO(SO4)2] are isostructural. VO6 octahedra with one terminal oxygen atom and pairs of sulfate tetrahedra form infinite chains by corner sharing. The chains are weakly interlinked to layers. The sulfate ions are distorted towards planar SO3 molecules and single oxygen atoms attached to vanadium. This structural detail gives an explanation for the mechanism of the reversible reaction K[VO(SO4)2] ⇄ K[VO2(SO4)] + SO3 at 400°C. Raman spectra of the compounds have been recorded and interpreted with respect to their structures.Crystal data: V2O3(SO4)2, monoclinic, space group P21/a, a = 947.2(4), b = 891.3(3), c= 989.1(4) pm, β = 104.56(3)°, Z = 4, 878 unique data, R(Rw) = 0.039(0,033); K[VO(SO4)2], orthorhombic, space group P212121, a = 495.3(2), b = 869.6(9), c = 1 627(1)pm, Z = 4, 642 unique data, R(Rw) = 0,11(0,10); NH4[VO(SO4)2], orthorhombic, space group P212121, a = 495.3(1), b = 870.0(2), c = 1 676.7(4)pm, Z = 4, 768 unique data, R(Rw) = 0.088(0.083).
    Notes: Die Oxo-sulfato-vanadate(V)V2O3(SO4)4, K[VO(SO4)2] und NH4[VO(SO4)2] wurden dargestellt und ihre Strukturen röntgenographisch ermittelt. Die Struktur von V2O3(SO4)2 besteht aus einem dreidimensionalen Netzwerk von SO4-Tetraedern und Paaren eckenverknüpfter VO6-Oktaeder. Die Sauerstoffatome der Sulfationen sind an vier verschiedene Vanadinatome koordiniert. K[VO(SO4)2] und NH4[VO(SO4)2] sind isostrukturell. VO6-Oktaeder, mit einem endständigen Sauerstoffatom, und Paare von SO4-Tetraedern sind über Ecken zu Ketten verknüpft. Diese bilden über weitere gemeinsame Ecken Schichten. Die Sulfationen sind in Richtung planarer SO3- Moleküle und eines Sauerstoffatoms, das an Vanadium gebunden ist, verzerrt. Dies gibt eine Erklärung für den Mechanismus der bei 400°C reversiblen Reaktion K[VO(SO4)2] ⇄ K[VO2(SO4)] + SO3. Die Ramanspektren der genannten Verbindungen wurden gemessen und zugeordnet.Kristalldaten: V2O3(SO4)2, monoklin, Raumgruppe P21/a, a = 947,2(4), b = 891,3(3), c = 989,1(4)pm, β = 104,56(3)°, Z = 4, 878 unabhängige Reflexe, R(Rw) = 0,039(0,033); K[VO(SO4)2], orthorhombisch, Raumgruppe P212121, a = 495,3(2), b = 869,6(9), c = 1627(1) pm, Z = 4, 642 unabhängige Reflexe, R(RW) = 0,11(0,10); NH4[VO(SO4)2], orthorhombisch, Raumgruppe P212121, a = 495,3(1), b = 870,0(2), c = 1676,7(4) pm, Z = 4, 768 unabhängige Reflexe, R(Rw) = 0, 088(0,083).
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926110526
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  • 7
    Electronic Resource
    Electronic Resource
    Komplexe offenkettiger und cyclischer Sulfoxide. Kristallstrukturen von CuII-, NiII-, PdII- und PtII-Komplexen des 3-Thia-1,5-diaminopentan-S-oxids und des 1-Thia-4,7-diazacyclononan-S-oxids (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 905-911 
    Details
    ISSN: 0044-2313
    Keywords: Complexes of Acyclic and Macrocyclic Sulfoxides ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complexes of Acyclic and Cyclic Sulfoxides. The Crystal Structures of CuII, NiII, PdII and PtII Complexes of 3-Thia-1,5-diaminopentane-S-oxide and 1-Thia-4,7-diazacyclononane-S-oxideThe macrocyclic ligand 1-thia-4,7-diazacyclononane-S-oxide (tasno) and the analogue acyclic ligand 3-thia-1,5-diaminopentane-S-oxide (daeso) have been prepared. Their reaction with the respective metal salts yielded the following compounds: [Ni(daeso)2](PF6)2 (1), [Pd(daeso)2](PF6)2 (2), [Cu(daeso)2]Cl2 (3), [Cu(daeso)2](ClO4)2 (4), [Cu(tasno)2]Br· 2 H2O (5), [Ni(tasno)2](ClO4)2 (6), [Pd(tasno)2]Br· H2O (7) and [Pt(tasno)2]Br· H2O (8). The structures of 1 and 4-8 have been determined by X-ray crystallography. In 4 and 5 CuII shows a Jahn-Teller distorted trans-N4O2 coordination, with O-donation of the sulfoxide group. O-donation of the SO-groups occurs also in the NiII complexes 1 and 6, giving a cis-N4O2 coordination sphere in 1 and a trans-N4O2 sphere in 6. In 7 the sulfur atom of the SO group is weakly interacting with the metal center in apical positions, whereas in 8 the sulfoxide group is directed away from the PdII ion. Metal to ligand distances in the complexes of tasno are shorter than in the complexes of daeso.
    Notes: Durch Oxidation von 1-Thia-4,7-diazacyclononan und 3-Thia-1,5-diaminopentan wurden der makrocyclische Ligand 1-Thia-4,7-diazacyclononan-S-oxid (tasno) und der entsprechende offenkettige Ligand 3-Thia-1,5-diaminopentan-S-oxid (daeso) dargestellt. Umsetzungen mit CuII-, NiII-, PdII- und PtII-Salzen ergaben die Komplexe [Ni(daeso)2](PF6)2 (1), [Pd(daeso)2](PF6)2 (2), [Cu(daeso)2]Cl2 (3), [Cu(daeso)2](ClO4)2 (4), [Cu(tasno)2]Br· 2 H2O (5), [Ni(tasno)2](ClO4)2 (6), [Pd(tasno)2]Br· H2O (7) und [Pt(tasno)2]Br· H2O (8). Die Strukturen von 1 und 4-8 wurden röntgenographisch anhand von Einkristallen ermittelt. In 4 und 5 ist CuII verzerrt oktaedrisch trans-N4O2 koordiniert, d. h. die Sulfoxidgruppen von tasno und daeso sind über die Sauerstoffatome gebunden. Dies ist auch in 1 und 6 der Fall, doch ist NiII in 1 cis-N4O2, in 6 dagegen trans-N4O2 koordiniert. In 7 besteht zusätzlich zur planaren PdN4-Koordination eine schwache Wechselwirkung zwischen Metallzentrum und dem Schwefelatom der Sulfoxidgruppe. In 8 ist die Sulfoxidgruppe vom Metallzentrum weggeklappt. Die Metall-Ligand-Abstände sind in den Komplexen des makrocyclischen Liganden tasno kürzer als in den Komplexen des offenkettigen Liganden daeso.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19936190518
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