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  • Articles: DFG German National Licenses  (47)
  • 1995-1999  (47)
  • Inorganic Chemistry  (47)
  • crystal structure  (10)
  • 1
    Electronic Resource
    Electronic Resource
    [Gd4(C2)](Cl, I)6, an Interstitially Stabilized Heteroleptic Gadolinium SesquihalideDedicated to Professor John D. Corbett on the Occasion of his 70th Birthday (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 494-500 
    Details
    ISSN: 0044-2313
    Keywords: Gadolinium sesquihalide ; interstitial carbon units ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Gd4(C2)](Cl, I)6, ein interstitiell stabilisiertes, heteroleptisches Gadoliniumsesquihalogenid[Gd4(C2)](Cl, I)6 erhält man aus CsI, Gd, GdCl3 und C2I4 in verschweißten Niob-Ampullen bei 1000/800°C in Form von schwarzen, glänzenden Nadeln. Die Kristallstruktur (tetragonal; P4/mbm; Z = 2; a = 1347,5(1); c = 1212,5(1) pm) ist ähnlich wie jene von Na[Mo4]O6 bzw. [Sc4B]Cl6. Trans-kantenverknüpfte [Gd6]-Oktaeder verlaufen parallel [001]. Sie enthalten interstitielle C2-Einheiten, Jedes dritte Oktaeder enthält fehlgeordnete C2-Einheiten, senkrecht zu jenen in den benachbarten [Gd6(C2)]-Oktaedern. Diese sind daher entlang der (pseudo)-C4-Achse gestaucht. Rechnungen zur elektronischen Struktur zeigen, daß insgesamt 13 Elektronen zur Auffüllung aller Metall-Metall-bindenden Zustände für eine „leere“ [Gd4]Cl6-Struktur nötig wären. Die Einlagerung der C2-Dimeren verändert die Bindungsverhältnisse in [Gd4(C2)]X6 (X = Cl, I) erheblich. Die formale Ladung von -6 der C2-Einheit wird durch das Aufsplitten der πg-Zustände reduziert, Gd—Gd und Gd—C-bindende Zustände werden besetzt und bindende dx2-y2-Orbitale kombinieren zu den am niedrigsten liegenden nicht besetzten Zuständen.
    Notes: [Gd4(C2)](Cl, I)6 is obtained from CsI, Gd, GdCl3 and C2I4 in sealed niobium containers at 1000/800°C as black, shiny needles. The crystal structure (tetragonal, P4/mbm, Z = 2, a = 1347.5(1), c = 1212.5(1) pm) is similar to that of Na[Mo4]O6 and [Sc4B]Cl6. It may be regarded as being built from octahedra sharing common trans edges running in the [001] direction. The octahedra contain C2 units as interstitials. Every third octahedron contains a disordered C2 unit perpendicular to those in the two neighboring [Gd6(C2)] octahedra and is therefore compressed in the direction of the (pseudo) C4 axis. Calculations of the electronic structure of an “empty” [Gd4]Cl6 structure reveals a total of 13 electrons necessary to occupy all metal-metal bonding states. The incorporation of a carbon dimer substantially alters the bonding conditions for [Gd4(C2)]X6 (X = Cl, I). The formal charge of -6 of the C2 unit is significantly reduced as πg states split up, Gd—Gd and Gd—C bonding states are occupied and bonding dx2—y2 orbitals combine to form the lowest unoccupied energy states.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220318
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  • 2
    Electronic Resource
    Electronic Resource
    Dimeric Silver(I) Complexes of Some Isothiazole-Based LigandsDedicated to Prof. Dr. Rolf Gleiter on the occasion of this 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 95-100 
    Details
    ISSN: 0009-2940
    Keywords: Isothiazole complexes ; Dinuclear silver(I) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of isothiazole-based potential ligands bearing substituents with additional donor sites in the 5-position of the heterocycle was synthesized [3-Me-5-R-C3HNS; R = CH=N(CH2)2py (1), CH=NCH2py (2), CH2N(CH2CH2NEt2)2 (4), (CH2)2SMe (5)]. Upon reaction with AgO3SCF3 they formed complexes [(1)AgOSO2CF3]2 (6), [(2)AgOSO2CF3]2 (7), [(4)Ag]2+2(O3SCF-3)2 (8) and [(5)AgOSO2CF3]2 (9), respectively. 6, 8 and 9 were shown by X-ray structural analyses to consist of dimeric units L2Ag2+2, either discrete (8), coordinated by terminal CF3SO-3 units (6). In 8 and 9 the isothiazole moiety is bonded to the metal center via the ring-N. The coordination potential of the isothiazole heterocycle is discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300115
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  • 3
    Electronic Resource
    Electronic Resource
    Pyrazolate-Based Oligonuclear Copper and Silver Complexes with N/S Coordination SpheresDedicated to Prof. Dr. Gottfried Huttner on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1441-1447 
    Details
    ISSN: 0009-2940
    Keywords: Pyrazolate complexes ; Bridging ligands ; Copper ; Silver ; N,S-Donor Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of pyrazole-based potential ligands bearing thioether substituents in 3- and 5-positions of the heterocycle was synthesized [3,5-bis(RSCH2)-pyzH R=Ph (1aH), PhCH2 (1bH), iPr (1cH), tBu (1dH)]. These ligands afford oligonuclear Cu1 and Ag1 coordination compounds [LCu]x (2a-c, L = 1a - c) and [LAg]x (3a-d, L = 1a-d), respectively. The single crystal X-ray analysis of 3c shows the presence of trimeric planar arrays of N,N′-bridging pyrazolates and linear coordinated silver ions, with each two of the trinuclear moieties being linked by two unsupported short intermolecular Ag…Ag contacts [3.041(1) Å]. Molecular-weight determinations for 2a (THF) and 3c (toluene) indicate that hexanuclear entities are preserved in solution. Starting from 1bH the CuII complex [(1b)2Cu2](BF4)2 (4) was synthesized. According to an X-ray crystal structure analysis it consists of dinuclear molecules with two bridging pyrazolates, distorted square planar N2S2 coordination spheres for Cu11 and an axially bridging tetrafluoroborate. Magnetic susceptibility data reveal an antiferromagnetic exchange (J = -206 cm-1) that is among the highest found for doubly pyrazolate bridged dicopper(II) complexes, which is rationalized on the basis of the rather symmetric dinuclear core of 4. The irreversibility of the electrochemical reduction and oxidation processes for the CuII and CuI compounds, respectively, is explained by the inability of the respective coordination framework to adapt to different geometric preferences.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301014
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  • 4
    Electronic Resource
    Electronic Resource
    Dinuclear Cobalt(II) Complexes of Pyrazole Ligands with Chelating Side ArmsDedicated to Prof. Dr. Walter Siebert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 605-613 
    Details
    ISSN: 0009-2940
    Keywords: Pyrazolate complexes ; Dinuclear complexes ; Bridging ligands ; Cobalt ; Conformational analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of pyrazole-based potential ligands bearing polydentate amine substituents in the 3- and 5-positions of the heterocycle has been synthesized [3,5-bis(R2NCH2)-pyzH R2N = Me2N(CH2)3NMe (2aH), [Me2N(CH2)3]2N (2bH), (Et2NCH2CH2)2N (2cH)]. Upon reaction with two equivalents of CoCl2 they form complexes LCo2Cl3 (3a-c; L = 2a-c, respectively) which are shown crystallographically to contain a dinuclear metal core bridged by both the pyrazolate unit and a chlorine atom, with each cobalt center carrying a further terminal chlorine atom. Two of the ligand side arms in 3b, c are dangling, thus leading to five-coordination of the cobalt(II) centers in all cases. Addition of two equivalents of NaBPh4 to solutions of 3b, c induced coordination of the formerly dangling side arms to the metal centers by substitution of the terminal chlorine atoms. The resulting compounds [LCo2Cl](BPh4)2 (4b, c, respectively) were characterized by X-ray structure analyses. They can be viewed as dinuclear linked versions of tran-type complexes [(tran = tris(aminoalkyl)amine] with distorted trigonal-bipyramidal coordination spheres around cobalt(II). Conformational analyses employing force-field calculations were carried out for 4b, c in order to rationalize the conformations observed in the solid state with regard to the accessible conformational space.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300511
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  • 5
    Electronic Resource
    Electronic Resource
    1,1-Hydroborierung von Alkinen mit 6-Aza-nido-decaboranen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 947-951 
    Details
    ISSN: 0009-2940
    Keywords: 6-Aza-nido-decaborane ; 9-(1-Alkenyl)-6-phenyl-6-aza-nido-decaborane ; 1,1-Hydroboration of alkynes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,1-Hydroboration of Alkynes with 6-Aza-nido-decaboranes[1]Alkynes AC≡CR′ (R′ = Me, Bu, tBu, SiMe3), that contain a mobile group A, like H or SiMe3, undergo hydroboration by 6-aza-nido-decaboranes RNB9H11 (1a-c, R = H, Ph, PhCH2) and 1,2-migration of the group A, to give the corresponding 9-(1-alkenyl)-6-aza-nido-decaboranes RNB9H10(CH=CR′A) (2a-h). Ethenes AHC=CH2 (A = SiMe3, SnBu3) are hydroborated by 1a, b as well to form products of the type RNB9H10(CH2CH2A) (3a-c). The alkyne Me3SiC=CH undergoes a hydroboration with 1b twice; the formation of (PhNB9H10)2CHCH2SiMe3 (4) proceeds by a 1,1- and a 1,2-hydroboration step, apparently. The crystal structure analysis of (PhCH2)NB9H10[CH=CMe(SiMe3)] (2e; space group Pl) reveals a (Z configuration of the ethene moiety.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280916
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  • 6
    Electronic Resource
    Electronic Resource
    Öffnung des Aza-closo-dodecaboran-Gerüsts durch Basen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1225-1229 
    Details
    ISSN: 0009-2940
    Keywords: 1-Organo-1-aza-closo-dodecaborane(12) ; Trialkylamine-1-organo-1-aza-nido-dodecaborane(12) (1/1) ; Undecahydro-1-organo-1-aza-nido-dodecaborate(1-), 2-hydro-, 2-halogeno-, 2-alkoxy-, 2-amino-, 2-alkyl- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Opening of the Aza-clso-dodecaborane Skeleton by BasesThe aza-closo-borane PhNB11H11 (1a) is opened by the amines NR3 (R = Me, Et) to give the novel aza-nido-dodecaboranes PhNB11H11(NR3) (2a, b). The non-planar open pentagonal face of 2a, b accomodates the N atom, a BHB bridge, and the base-bound B atom, according to NMR spectra and the crystal structure analysis of monoclinic 2b. A similar but more symmetric structure is found when closo-RNB11H11 (1a-c, R = Ph, Me, H) is attacked by anionic bases X- to give nido-RNB11H11X- (3a-j; R/X = Me/H, Me/F, Me/Cl, Ph/OH, H/OMe, Me/OMe, Me/OtBu, Me/NEt2, Me/Me, Me/Bu). The anions are precipitated with cations [K([18]crown-6)], [S(NMe2)3], [N(PPh3)2], [Et2NH2], or [Li(tmeda)2]. The nido-structures of type 2 and 3 are derived from the hypothetical closo-NB12H13.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281214
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  • 7
    Electronic Resource
    Electronic Resource
    Ternäre Halogenide vom Typ A3MX6. IV. [1]. Ternäre Halogenide des Scandiums mit Natrium, Na3ScX6 (X = F, Cl, Br): Synthese, Strukturen, IonenleitfähigkeitIn memoriam Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 173-178 
    Details
    ISSN: 0044-2313
    Keywords: Scandium ; Halides ; Crystal Structures ; Ionic Conductivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Halides of the A3MX6 Type. IV. Ternary Halides of Scandium with Sodium, Na3ScX6 (X = F, Cl, Br): Synthesis, Structures, Ionic ConductivityX-ray studies on single crystals of Na3ScF6 and Na3ScBr6 show, that Na3ScF6 crystallizes with the cryolite type (monoclinic, P21/n, Z = 2, a = 560.16(9), b = 580.31(8), c = 812.1(2)pm, β = 90.720(14)°) and Na3ScBr6, as the only ternary bromide of the rare earth elements with sodium, in the Na3CrCl6 type (trigonal, P31c, Z = 2, a = 728.95(7), c = 1309.29(17)pm). The ionic conductivity of powder samples of Na3ScF6, Na3ScBr6 and of Na3ScCl6 was studied by impedance spectroscopy. Activation energies were determined as 1.22 eV, 0.80 eV and 0.71 eV for the fluoride, chloride and bromide, respectively. The differences are explained from the crystal structures and the sizes and polarizabilities of the anions.
    Notes: Röntgenographische Untersuchungen an Einkristallen von Na3ScF6 und Na3ScBr6 ergaben, daß Na3ScF6 im Kryolith-Typ (monoklin, P21/n, Z = 2, a = 560,16(9), b = 580,31(8), c = 812,1(2)pm, β = 90,720(14)°) und Na3ScBr6 als bisher einziges ternäres Bromid der Selten-Erd-Elemente mit Natrium im Na3CrCl6-Typ (trigonal, P31c, Z = 2, a = 728,95(7), c = 1309,29(17)pm) kristallisieren. An Pulverproben von Na3ScF6 und Na3ScBr6 sowie an Na3ScCl6 wurden Leitfähigkeitsuntersuchungen mittels Impedanzspektroskopie vorgenommen und aus den Ergebnissen die Aktivierungsenergien für den Leitungsprozeß zu 1,22 eV, 0,80 eV und 0,71 eV für das Fluorid, Chlorid bzw. Bromid bestimmt. Die Unterschiede werden aus den Kristallstrukturen sowie durch die Größen und Polarisierbarkeiten der Anionen erklärt.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220125
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  • 8
    Electronic Resource
    Electronic Resource
    Phosphaniminato-Komplexe von Cobalt und Zink mit Heterocubanstruktur. Die Kristallstrukturen von [CoI(NPMe3)]4 und [ZnI(NPMe3)]4 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 867-872 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes ; Cobalt ; Zinc ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Cobalt and Zinc with Heterocubane Structure. Crystal Structures of [CoI(NPMe3)]4 and [ZnI(NPMe3)]4The title compounds have been prepared from CoI2 and ZnI2, respectively, and Me3SiNPMe3 by fusion reactions at 180°C in the presence of sodium fluoride. They crystallize from dichloromethane as dark green (Co) or colourless (Zn) single crystals including three molecules CH2Cl2 per formula unit, which were characterized by crystal structure determinations. [CoI(NPMe3)]4 · 3 CH2Cl2: Space group P3m1, Z = 2, structure solution with 2376 independent reflections, R = 0.033. Lattice dimensions at -50°C: a = b = 1455.8, c = 1270.5 pm.[ZnI(NPMe3)]4 · 3 CH2Cl2: Space group P3m1, Z = 2, structure solution with 2197 independent reflections, R = 0.043. Lattice dimensions at -60°C: a = b = 1454.9, c = 1270.5 pm. Both complexes are isostructural with one another. They form heterocubane structures in which the metal atoms are linked via μ3-N-bridges of the phosphoraneiminato groups with M4N4 bridge-type bond angles close to 90°.
    Notes: Die Titelverbindungen werden durch Reaktionen von CoI2 bzw. ZnI2 mit dem silylierten Phosphanimin Me3SiNPMe3 durch Schmelzreaktion bei 180°C in Gegenwart von Natriumfluorid synthetisiert. Sie kristallisieren aus Dichlormethan als dunkelgrüne (Co) bzw. farblose (Zn) Einkristalle mit drei Molekülen Dichlormethan pro Formeleinheit, die wir durch Kristallstrukturanalysen charakterisiert haben. [CoI(NPMe3)]4 · 3 CH2Cl2: Raumgruppe P3m1, Z = 2, Strukturlösung mit 2376 unabhängigen Reflexen, R = 0,033. Gitterkonstanten bei -50°C: a = b = 1455,8; c = 1270,5 pm.[ZnI(NPMe3)]4 · 3 CH2Cl2: Raumgruppe P3m1, Z = 2, Strukturlösung mit 2197 unabhängigen Reflexen, R = 0,043. Gitterkonstanten bei -60°C: a = b = 1454,9; c = 1270,5 pm. Die beiden miteinander isotypen Verbindungen bilden Heterocuban-Strukturen, in denen die Metallatome über μ3-N-Brücken der Phosphaniminato-Gruppen verknüpft sind mit M4N4-Brückenbindungswinkeln nahe bei 90°.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220520
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  • 9
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    Electronic Resource
    [La2I2(OH)2(Dibenzo-18-Krone-6)2]I(I3), ein kationischer, dimerer in-cavity-Komplex mit Iodid und Triiodid als Anionen (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1493-1495 
    Details
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Crown ether ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3), a Cationic Dimeric in-cavity Complex with Iodide and Triiodide as AnionsSingle crystals of [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3) are obtained from the reaction of LaI3 and dibenzo-18-crown-6 in acetonitrile. The crystal structure monoclinic, C2/m, Z = 4, T = 293 [100] K, a = 2179(3) [2162.3(3)], b = 1070.3(3) [1069.6(1)], c = 1118.2(3) [1110.6(1)] pm, β = 93.1(1) [92.83(1)]°, R1 = 0.0601 [0.0411], wR2 = 0.1449 [0.1014] contains hydroxide-bridged cationic dimers and iodide as well as triiodide as anions.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231002
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  • 10
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    Electronic Resource
    Synthese und Kristallstruktur von NH4DyF4. Über weitere Fluoride NH4MF4 (M = La—Tb) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1393-1398 
    Details
    ISSN: 0044-2313
    Keywords: Rare Earth Fluorides ; Crystal Structure ; Ammonium Fluorides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of NH4DyF4. Further Fluorides NH4MF4 (M = La—Tb)
    Notes: Die Fluoride NH4MF4 (M = La—Dy) entstehen bei der Umsetzung der Metalle M mit N2H6F2 bei Temperaturen zwischen 80 und 350°C in verschweißten Monelampullen. Es werden in Abhängigkeit vom Selten-Erd-Element und von der Reaktionstemperatur drei Strukturen beobachtet: Die Kristallstruktur der Form I wurde anhand von Einkristallen von NH4DyF4 aufgeklärt [orthorhombisch, Pbcm (Nr. 57), Z = 4; a = 852,10(7) pm, b = 722,54(8) pm, c = 626,28(12) pm]; die bei niedrigen Temperaturen hergestellten Fluoride NH4MF4 (M = Ce—Tb) sind isotyp. Bei höheren Temperaturen treten die Formen II [für M = La—Nd; orthorhombisch (?), Z = 8] bzw. III [M = Eu—Tb, geordnete Überstruktur zum CaF2-Typ, analog TlGdF4, tetragonal, P4/m (?), Z = 16] auf.The fluorides NH4MF4 (M = La—Dy) are obtained through the reaction of the metals M with N2H6F2 at temperatures between 80 and 350°C in sealed Monel ampoules. Dependent upon the rare-earth element M and the reaction temperature three crystal structures are observed: The crystal structure of modification I was determined from single crystal data of NH4DyF4 [orthorhombic, Pbcm (no. 57), Z = 4; a = 852.10(7) pm, b = 722.54(8) pm, c = 626.28(12) pm]; the fluorides NH4MF4 (M = Ce—Tb) obtained at fairly low temperatures are isotypic. At higher temperatures the modifications II [for M = La—Nd; orthorhombic (?), Z = 8] and III [M = Eu—Tb, ordered superstructure of the CaF2 type, analogous to TlGdF4, tetragonal, P4/m (?), Z = 16] are observed.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230913
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