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  • 1
    Electronic Resource
    Electronic Resource
    Organotin(IV) complexes with tetraethyl ethylene- and propylene-diphosphonates (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 9 (1995), S. 11-22 
    Details
    ISSN: 0268-2605
    Keywords: organotin(IV) complexes ; diphosphoryl ligands ; NMR ; Mössbauer spectroscopy ; X-ray analysis ; antitumour activity ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The series of organotin halide complexes with tetraethyl ethylene- and propylene-diphosphonates RnSnX4-n,·L [n=0, X=Cl; n=1, R=Me, X=Cl, Br; n=1, R=Ph, X=Cl; n=2, R=Me, Et, Bu, X=Cl, Br; n=2, R=Ph, X=Cl; L=(EtO)2P(O)CH2CHR'P(O)(OEt)2, R'=H, Me] were synthesized and characterized by means of NMR and Mössbauer spectroscopy. The crystal structure of the complex of diphenyltin dichloride with propylenediphosphonate was determined. The complex consists of polymer chains with bridging bidentate ligands and an octahedral tin environment containing two types of phosphoryl fragments. All of the R2SnX2 adducts have trans-R2SnX4 geometries of tin coordination octahedra according to the quadrupole splitting values in the Mössbauer spectra. The 31P and 119Sn NMR studies at low temperatures revealed that RSnHal3 complexes in solution form isomers with different mutual orientations of phosphoryl ligands and organic groups in the coordination sphere. The diethyltin dichloride adduct with ethylene-diphosphonate appeared to be active against lung cancer NCI-H522 cells.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/aoc.590090104
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  • 2
    Electronic Resource
    Electronic Resource
    Combining oxidative addition and polymerization: A study towards the synthesis of macromonomers (1997)
    Weinheim : Wiley-Blackwell
    Acta Polymerica 48 (1997), S. 432-437 
    Details
    ISSN: 0323-7648
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Oxidative addition to a metal in a low valent state produces catalysts that allow reporter or functional groups to be introduced to a polymer chain end. Substituted allyltrifluoroacetates were added to Ni(0)(COD)2. The resulting π-allyl-Ni trifluoroacetates are dimeric in the solid state as well as in solution. The crystal structure of bis[(η3-2-phenylallyl)(trifluoroacetato)-nickel(II)], bis[(η3-2-trimethylsilylallyl)(trifluoroacetato)nickel(II)], are given and correlated with the reactivity as polymerization catalysts. Butadiene, styrene, and norbornene are used as monomers. The substituent of the allyl group is found quantitatively to be the end group of each macromolecule. Thus it is demonstrated that no chain transfer occurs.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/actp.1997.010481003
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  • 3
    Electronic Resource
    Electronic Resource
    Phosphanimin- und Phosphaniminato-Komplexe von Eisen. Die Kristallstrukturen von [FeCl3(Me3SiNPEt3)], [FeCl2(Me3SiNPEt3)]2, [FeCl2(NPEt3)]2 und [Fe(O2C—CH3)2(NPEt3)]2Professor Erwin Hellner zum 75. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 705-712 
    Details
    ISSN: 0044-2313
    Keywords: Phosphanimine ; Phosphoraneiminato Complexes of Iron ; Syntheses ; IR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphanimine and Phosphoraneiminato Complexes of Iron. The Crystal Structures of [FeCl3(Me3SiNPEt3)], [FeCl2(Me3SiNPEt3)]2, [FeCl2(NPEt3)]2, and [Fe(O2C—CH3)2(NPEt3)]2The phosphanimine complexes [FeCl3(Me3SiNPEt3)] (red-orange) and [FeCl2(Me3SiNPEt3)]2 (colourless) have been prepared by reactions of Me3SiNPEt3 with FeCl3 and FeCl2, respectively, in CH2Cl2 suspensions. Thermal decomposition of these donor-acceptor complexes in boiling toluene leads to the phosphoraneiminato complex [FeCl2(NPEt3)]2 (black), whereas [Fe(O2C—CH3)2(NPEt3)]2 (brown) is formed from iron(II) acetate and Me3SiNPEt3 in boiling acetonitrile. The complexes are characterized by IR spectroscopy and by crystal structure determinations.[FeCl3(Me3SiNPEt3)] (1): Space group P21/c, Z = 8, structure determination with 4 673 unique reflections, R = 0.033. Lattice dimensions at -15°C: a = 1 607.8, b = 1 602.0, c = 1 417.2 pm, β = 106.56°. 1 forms monomeric molecules with tetrahedrally coordinated iron atoms. Bond lengths in average: Fe—N = 196.9 pm, Fe—Cl = 219.7 pm.[FeCl2(Me3SiNPEt3)]2 (2): Space group P21/c, Z = 4, structure determination with 4 992 unique reflections, R = 0.048. Lattice dimensions at 20°C: a = 1 457.9, b = 1 685.4, c = 1 507.3 pm, β = 116.74°. 2 forms dimeric molecules, which are associated by chloro bridges. The iron atoms are tetrahedrally coordinated with trans positions of the phosphanimine ligands. Both lengths in average: Fe—N = 202.2 pm, Fe—Clterminal = 224.7 pm, Fe—Clbridge = 241.0 pm.[FeCl2(NPEt3)]2 (3): Space group P21/n, Z = 2, structure determination with 2763 unique reflections, R = 0.039. Lattice dimensions at -70°C: a = 799.1, b = 1009.0, c = 1441.9 pm, β = 93.45°. 3 forms centrosymmetric dimeric molecules, in which the tetrahedrally coordinated iron atoms are associated by the nitrogen atoms of the phosphoraneiminato ligands. Bond lengths in average: Fe—N = 191.4 pm, Fe—Cl = 222.7 pm.[Fe(O2C—CH3)2(NPEt3]2 (4): Space group P21/n, Z = 2, structure determination with 3005 observed unique reflections, R = 0.034. Lattice dimensions at -65°C: a = 886.4, b = 1444.6 pm, β = 90.60°. 4 forms centrosymmetric dimeric molecules, in which the octahedrally coordinated iron atoms are associated by the nitrogen atoms of the phosphoraneiminato ligands with bond lengths Fe—N of 191.9 and 195.0 pm. The acetate groups are coordinated in a chelating fashion.
    Notes: Die Phosphanimin-Komplexe [FeCl3(Me3SiNPEt3)] (rotorange) und [FeCl2(Me3SiNPEt3)]2 (farblos) entstehen durch Reaktion von FeCl3 bzw. FeCl2 mit Me3SiNPEt3 in CH2Cl2-Suspensionen. Erhitzen dieser Donor-Akzeptorkomplexe in Toluol führt zu dem Phosphaniminatoderivat [FeCl2NPEt3)]2 (schwarz), während [Fe(O2C—CH3)2 · (NPEt3)]2 (braun) aus Eisen(II)-acetat und Me3SiNPEt3 in siedendem Acetonitril entsteht. Die Komplexe werden durch die IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[FeCl3(Me3SiNPEt3)] (1): Raumgruppe P21/c, Z = 8, Strukturlösung mit 4 673 unabhängigen Reflexen, R = 0,033. Gitterkonstanten bei -15°C: a = 1 607,8; b = 1 602,0; c = 1 417,2 pm, β = 106,56°. 1 hat eine monomere Molekülstruktur mit tetraedrisch koordiniertem Eisenatom und mittleren Bindungslängen Fe—N = 196,9 pm, Fe—Cl = 219,7 pm.[FeCl2(Me3SiNPEt3)]2 (2): Raumgruppe P21/c, Z = 4, Strukturlösung mit 4 992 unabhängigen Reflexen, R = 0,048. Gitterkonstanten bei 20°: a = 1 457,9; b = 1 685,4; c = 1 507,3 pm, β = 116,74°. 2 bildet dimere, über Chlorobrücken assoziierte Moleküle mit tetraedrisch koordinierten Eisenatomen und trans-Stellung der Phosphanimin-Liganden. Mittlere Bindungslängen: Fe—N = 202,2 pm, Fe—Clterminal = 224,7 pm, Fe—ClBrücke = 241,0 pm.[FeCl2(NPEt3)]2 (3): Raumgruppe P21/n, Z = 2, Strukturlösung mit 2 763 unabhängigen Reflexen, R = 0,039. Gitterkonstanten bei -70°C: a = 799,1; b = 1 009,0; c = 1 441,9 pm, β = 93,45°. 3 bildet zentrosymmetrische dimere Moleküle, in denen die tetraedrisch koordinierten Eisenatome über die N-Atome der Phosphaniminatoliganden assoziiert sind. Mittlere Bindungslängen: Fe—N = 191,4 pm, Fe—Cl = 222,7 pm.[Fe(O2C—CH3)2(NPEt3)]2 (4): Raumgruppe P21/n, Z = 2, Strukturlösung mit 3 005 unabhängigen beobachteten Reflexen, R = 0,034. Gitterkonstanten bei -65°C: a = 886,4; b = 1 112,7; c = 1 444,6 pm; β = 90,60°. 4 bildet zentrosymmetrische dimere Moleküle, in denen die oktaedrisch koordinierten Eisenatome über die N-Atome der Phosphaniminatoliganden mit Fe—N-Abständen von 191,9 und 195,0 pm assoziiert sind. Die Acetatgruppen sind chelatartig gebunden.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210502
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  • 4
    Electronic Resource
    Electronic Resource
    Phosphaniminato-Komplexe von Mangan(II) und Nickel(II) mit Heterocubanstruktur. Die Kristallstrukturen von [MCl(NPEt3)]4 mit M = Mn und NiProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1963-1968 
    Details
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes of Manganese and Nickel ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Manganese(II) and Nickel(II) with Heterocubane Structure. Crystal Structures of [MCl(NPEt3)]4 with M = Mn and NiThe phosphoraneiminato complexes [MCl(NPEt3)]4 with M = manganese and nickel as well as [MnBr(NPEt3)]4 are formed from the anhydrous halides MX2 and excess phosphoraneimine Me3SiNPEt3 by fusion reaction. They form paramagnetic, moisture-sensitive, orange (M = Mn) and turquoisegreen (M = Ni) crystals, respectively, which are characterized by i.r. spectroscopy and by crystal structure determinations.[MnCl(NPEt3)]4 (1): Space group C2/c, Z = 4, structure solution with 3 591 unique reflections, (2 811 〉 2σ(I)) R = 0.036. Lattice dimensions at -50°C: a = 2104.3, b = 1100.6, c = 1966.5 pm, β = 115.87°.[NiCl(NPEt3)]4 (2): Space group C2/c, Z = 4, structure solution with 2 711 unique reflections, (1611 〉 2σ(I)) R = 0.056. Lattice dimensions at -50°C: a = 2051.6, b = 1099.2, c = 1954.6 pm, β = 115.80°.1 and 2 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 Phosphaniminato-Komplexe [MCl(NPEt3)]4 mit M = Mangan und Nickel sowie [MnBr(NPEt3)]4 entstehen durch Schmelzreaktion aus den wasserfreien Halogeniden MX2 und überschüssigem Phosphanimin Me3SiNPEt3. Sie bilden paramagnetische, feuchtigkeitsempfindliche, orange (M = Mn) bzw. türkisgrüne (M = Ni) Kristalle, die wir IR-spektroskopisch und durch Kristallstrukturanalysen charakterisiert haben. [MnCl(NPEt3)]4 (1): Raumgruppe C2/c, Z = 4, Strukturlösung mit 3 591 unabhängigen Reflexen, (2811 〉 2σ(I)) R = 0,036. Gitterkonstanten bei -50°C: a = 2104,3; b = 1100,6; c = 1966,5 pm, β = 115,87°.[NiCl(NPEt3)]4 (2): Raumgruppe C2/c, Z = 4, Strukturlösung mit 2 771 unabhängigen Reflexen, (1 611 〉 2σ(I)) R = 0,056. Gitterkonstanten bei -50°C: a = 2051,6; b = 1 099,2; c = 1954,6 pm, β = 115,80°.1 und 2 sind miteinander isotyp. Sie 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.19956211122
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Seltenerd-Komplexe [LaI2(THF)5]+I3-, [SmCl3(THF)4], [ErCl2(THF)5]+ [ErCl4(THF)2]-, [ErCl3(DME)2] und [Na(18-Krone-6)(THF)2]+ [YbBr4(THF)2]- (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1425-1432 
    Details
    ISSN: 0044-2313
    Keywords: Rare-Earth Complexes ; Syntheses ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Rare-Earth Complexes [LaI2(THF)5]+I3-, [SmCl3(THF)4], [ErCl2(THF)5]+ [ErCl4(THF)2]-, [ErCl3(DME)2], and [Na(18-Crown-6)(THF)2]+[YbBr4(THF)2]-[LaI2(THF)5]+I3- (1) is obtained as red crystals from lanthanum powder and 1,2-diiodoethane in THF on exposure to light. Space group Pbcn, Z = 4, lattice dimensions at -83°C: a = 1264.9, b = 2218.9, c = 1199.1 pm, R = 0.031. The lanthanum atom of the cation of 1 is coordinated with iodine atoms in the axial positions in a pentagonal-bipyramidal way.[SmCl3(THF)4] (2) originates as colourless crystals on heating SmCl3 with excess THF in the presence of Me3SiNPEt3. Space group P21/c, Z = 8, lattice dimensions at -50°C: a = 3092.7, b = 826.2, c = 1758.3 pm, β = 93.85°, R = 0.054. Just like the known sample that crystallizes within the space group F2dd, 2 forms monomeric molecules in which the samarium atom is coordinated with two chlorine atoms in the axial positions in a distorted pentagonal-bipyramidal way.[ErCl2(THF)5]+[ErCl4(THF)2]- (3). Pale pink single crystals of 3 were prepared according to the described method by reaction of erbium powder with trimethylchlorosilane and methanol in THF. Space group C2/c, Z = 4, lattice dimensions at -50°C: a = 1246.3, b = 1145.7, c = 2726.0 pm, β = 91.293°, R = 0.036. The erbium atom of the cation of 3 has a pentagonal-bipyramidal coordination with the chlorine atoms in the axial positions. Within the anion the THF molecules are in trans-arrangement of the octahedrally coordinated erbium atom.[ErC13(DME)2] (4) originates as pink single crystals from 3 with excess boiling 1,2-dimethoxyethane. Space group P21/c, Z = 4, lattice dimensions at -50°C: a = 1137.2, b = 886.5, c = 1561.1 pm, β = 104.746°, R = 0.032. 4 forms monomeric molecules in which the erbium atom has a pentagonal-bipyramidal surrounding with two chlorine atoms in the axial positions.[Na(18-Krone-6)(THF)2]+ [YbBr4(THF)2]- (5) is formed as by-product by the reaction of YbBr3 with NaN(SiMe3)2 in THF in the presence-of 18-crown-6 forming colourless crystals. Space group P1, Z = 1, lattice dimensions at -70°C: a = 934.6, b = 988.9, c = 1208.0 pm, α = 73.82°, β = 72.98°, γ = 76.89°, R = 0.029. 5 contains isolated [YbBr4(THF)2]-ions, in which the THF molecules are arranged in trans-position.
    Notes: [LaI2(THF)5]+I3- (1) wird aus Lanthanpulver und 1,2-Diiodethan in THF unter Lichteinwirkung als rote Kristalle erhalten. Raumgruppe Pbcn, Z = 4, Gitterkonstanten bei -83°C: a = 1264,9; b = 2218,9; c = 1199,1 pm; R = 0,031. Das Lanthanatom des Kations von 1 ist pentagonal-bipyramidal koordiniert mit den Iodatomen in den Axialpositionen.[SmCl3(THF)4] (2) entsteht beim Erhitzen von SmCl3 mit überschüssigem THF in Gegenwart von Me3SiNPEt3 als farblose Einkristalle. Raumgruppe P21/c, Z = 8, Gitterkonstanten bei -50°C: a = 3092,7; b = 826,2; c = 1758,3 pm; β = 93,85°; R = 0,054. 2 bildet wie das bereits bekannte, in der Raumgruppe F2dd kristallisierende Präparat, monomere Moleküle, in denen das Samariumatom verzerrt pentagonal-bipyramidal koordiniert ist mit zwei Chloratomen in den Axialpositionen.[ErCl2(THF)5]+ [ErCl4(THF)2]- (3). Blaßrosa Einkristalle von 3 erhielten wir nach der literaturbekannten Methode durch Reaktion von Erbiumpulver mit Trimethylchlorsilan und Methanol in THF. Raumgruppe C2/c, Z = 4, Gitterkonstanten bei -50°C: a = 1246,3; b = 1145,7; c = 2726,0 pm; β = 91,293°; R = 0,036. Das Erbiumatom des Kations von 3 hat pentagonal-bipyramidale Koordination mit den Chloratomen in den Axialpositionen, im Anion befinden sich die THF-Moleküle in der trans-Anordnung des oktaedrisch koordinierten Erbiumatoms.[ErCl3(DME)2] (4) entsteht als rosa Einkristalle aus 3 mit überschüssigem, siedendem 1,2-Dimethoxyethan. Raumgruppe P21/c, Z = 4, Gitterkonstanten bei -50°C: a = 1137,2; b = 886,5; c = 1561,1 pm; β = 104,746°; R = 0,032. 4 bildet monomere Moleküle, in denen das Erbiumatom verzerrt pentagonal-bipyramidale Umgebung hat mit zwei Chloratomen in den Axialpositionen.[Na(18-Krone-6)(THF)2]+ [YbBr4(THF)2]- (5) entsteht als Begleitprodukt bei der Umsetzung von YbBr3 mit NaN(SiMe3)2 in THF in Gegenwart von 18-Krone-6 als farblose Kristalle. Raumgruppe P1, Z = 1, Gitterkonstanten bei -70°C: a = 934,6; b = 988,9; c = 1208,0 pm; α = 73,82°; β = 72,98°; γ = 76,89°; R = 0,029. 5 enthält isolierte [YbBr4(THF)2]--Ionen, in denen die THF-Moleküle in trans-Stellung angeordnet sind.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230918
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  • 6
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    Electronic Resource
    Phosphaniminato-Komplexe des Schwefels. Kristallstrukturen von [S(NPEt3)3]Cl, [S(NPEt3)2]Cl2 und [Me3SiOSO2NPPh3] (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 962-966 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes ; Sulfur Compounds ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Sulfur. Crystal Structures of [S(NPEt3)3]Cl, [S(NPEt3)2]CI2 and [Me3SiOSO2NPPh3]The ionic phosphorane iminato complexes [S(NPEt3)3]Cl and [S(NPEt3)2]Cl2 are obtained as colourless, moisture sensitive crystals after reaction of Me3SiNPEt3 with disulfur dichloride from acetonitrile solutions. Both complexes, as well as the molecular complex [Me3SiOSO2NPPh3]. which is known from literature data, were characterized by crystal structure determinations.
    Notes: Die ionisch aufgebauten Phosphaniminato-Komplexe [S(NPEt3)3]Cl und [S(NPEt3)2]Cl2 entstehen als farblose, feuchtigkeitsempfindliche Kristalle nach Reaktion von Me3SiNPEt3 mit Dischwefeldichlorid in Acetonitrillösung. Beide Komplexe werden ebenso wie die literaturbekannte Molekülverbindung [Me3SiOSO2NPPh3] durch Kristallstrukturanalysen charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.199762301150
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  • 7
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    Electronic Resource
    Die Struktur der Fluoridhydrate CoAlF5 · 7 H2O und MnFeF5 · 7 H2OProfessor Walter Rüdorff in memoriam (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 579 (1989), S. 191-199 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Structure of the Fluoride Hydrates CoAlF5 · 7H2O and MnFeF5 · 7H2OSingle crystals of fluoride hydrates CoAlF5 · 7H2O and MnFeF5 · 7H2O have been prepared and characterized by X-ray methods. The Co/Al compound crystallizes in space group C2/m (a = 1091.7(7), b = 1386.3(14), c = 652.5(6) pm, β = 100.30(6)°, Z = 4). H2O/F- disorder occurs over two trans positions in the ligand sphere of Al3+, whereas the Mn/Fe compound shows an ordered variety with [FeF6]3- and [FeF4(H2O)2]- anions crystallizing in space group C2/c (a = 1118.2(3), b = 1416.8(4), c = 1326.4(3) pm, β = 100.51(2)°, Z = 8). Both structures exhibit strong hydrogen bonds between [MII(H2O)6]2+ cations and the fluorine ligands in the coordination sphere around the tervalent metals. The complex cations and anions are grouped like in CsCl type salts.
    Notes: Erstmals wurden die Fluoridhydrate CoAlF5 · 7H2O und MnFeF5 · 7H2O in einkristalliner Form präpariert und röntgenographisch untersucht. Die Co/Al-Verbindung kristallisiert in der Raumgruppe C2/m (a = 1091,7(7), b = 1386,3(14), c = 652,5(6) pm, β = 100,30(6)°, Z = 4) mit H2O/F--Fehlordnung auf 2 trans-ständigen Lagen in der Al3+-Koordinationssphäre, wogegen die Mn/Fe-Verbindung eine geordnete Variante mit den Anionen [FeF6]3- und [FeF4(H2O)2]- in Raumgruppe C2/c bildet (a = 1118,2(3), b = 1416,8(4), c = 1326,4(3) pm, β = 100,51(2)°, Z = 8). Beiden Strukturen gemeinsam sind starke Wasserstoffbrückenbindungen zwischen den [MII(H2O)6]2+-Kationen einerseits und der Fluoridkoordinationssphäre der dreiwertigen Metalle andererseits. Die komplexen Kationen und Anionen sind wie im CsCl-Typ angeordnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19895790122
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  • 8
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    Electronic Resource
    Wasserstoffbrücken in fluoridhaltigen Festkörpern. I. Darstellung, Eigenschaften und Kristallstruktur von (NH4)2 [Cr(H2O)6]F5 (1977)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 436 (1977), S. 29-38 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Bonds in Fluorine Containing Solids. I. Preparation, Properties, and Crystal Structure of (NH4)2[Cr(H2O)6]F5The new red chromium(III) fluorine compound diammonium hexa-aqua chromium(III) pentafluoride has been prepared from solution and investigated by spectroscopic and magnetic methods. Single crystal investigations showed a monoclinic unit cell with hexagonal metric (space group C2/c): a = 11.997(1) Å, b = 6.928(1) Å, c = 13.574(2) Å, β = 90.0° (a = b √3). As result of the X-ray structure determination (Rw = 0.023) we found three dimensional connexion of nearly regular [Cr(H2O)6]-octahedra by  - O—H … F … H—O-type H bonds and an additional bridging between the F- ions by H bonds to the NH4+ ions. The NH4+ ions as well as the F- ions have tetrahedral coordination. Three different species of tetrahedral groups: [NH4(F4)], [F(NH4(H2O)3)], and [F((H2O)2(NH4)2)] may be distinguished. All hydrogen bonds are nearly linear and show very short distances O—F (2.53-2.57 Å) and N—F (2.72-2.73 Å). This novel three dimensional network of H bonds stabilizes apparently the [Cr(H2O)6] complex despite the presence of “free” fluorine ions in the crystal.
    Notes: Die neue rote Chrom(III)-Fluor-Verbindung Diammonium-hexaaquochrom(III)-pentafluorid wurde aus Lösung dargestellt und spektroskopisch sowie magnetisch untersucht. Einkristalluntersuchungen ergaben eine monokline Elementarzelle mit hexagonaler Metrik (Raumgruppe C2/c): a = 11,997(1) Å, b = 6,928(1) Å, c = 13,574(2) Å, β = 90,0°(a = b √3). Die Röntgenstrukturanalyse (Rw = 0,023) zeigte dreidimensionale Verknüpfung von nahezu regulären [Cr(H2O)6]-Oktaedern über - O—H … F … H—O-Wasserstoffbrücken und zusätzliche Verbrückung der F--Ionen über H-Brücken zu den NH4+-Ionen. Sowohl die NH4+-wie die F--Ionen sind dabei tetraedrisch koordiniert, wobei sich drei verschiedene Baugruppen: [NH4(F4)], [F(NH4(H2O)3)] und [F((NH4)2(H2O)2)] formulieren lassen. Alle H-Brücken sind nahezu linear und zeigen sehr kurze O—F-Abstände von 2,53-2,57 Å und N—F-Abstände von 2,72-2,73 Å. Dieses neuartige System von H-Brücken stabilisiert offenbar den [Cr(H2O)6]-Komplex trotz der Anwesenheit “freier” F--Ionen im Kristall.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19774360103
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  • 9
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    Reaktionen von Chloronitrenkomplexen des Molybdäns und Wolframs mit Silberfluorid Die Kristallstruktur von AsPh4[WOF5] (1982)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 493 (1982), S. 33-40 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Chloro-nitrene Complexes of Molybdenum and Tungsten with Silver Fluoride. Crystal Structure of AsPh4[WOF5]The reaction of AsPh4[Cl5Mo≡N—CCl3] with silver fluoride in acetonitrile gives by cleavage of the nitrene ligand AsPh4[MoOF5] as well as AsPh4[cis-MoF2Cl4] in the form of red-brown, very sensitive crystals. The analogous reaction with the tungsten complex AsPh4[Cl5W≡N—CCl3] yields the perfluorinated nitrene complex AsPh4[F5W≡N—CF3] apart from AsPh4[WOF5]. All products are characterised by i.r. spectroscopy.By aid of X-ray diffraction, the crystal structure of AsPh4[WOF5] was determined. The compound crystallizes in the tetragonal space group I4 with two formula units per unit cell (975 independent reflexions, R = 0.052). The [WOF5]⊖ anion has the point symmetry 4, indicating disorder. Least squares refinement of the model, taking into account split positions, shows the WO bond to contain significant π-bonding, which results in a displacement of the F atoms from the equatorial plane (  OWFeq. = 96.4°).
    Notes: Die Umsetzung von AsPh4[Cl5Mo≡N—CCl3] mit Silberfluorid in Acetonitril führt in komplexer Reaktion unter Abspaltung des Nitrenliganden neben AsPh4[MoOF5] zur Darstellung von AsPh4[cis-MoF2Cl4], welches rotbraune, sehr empfindliche Kristalle bildet. Bei der analogen Reaktion mit dem Wolframkomplex AsPh4[Cl5W≡N—CCl3] läßt sich neben AsPh4[WOF5] der perfluorierte Nitrenkomplex AsPh4[F5W≡N—CF3] erhalten. Die Präparate werden IR-spektroskopisch charakterisiert.Mittels Röntgenbeugung wurde die Kristallstruktur des AsPh4[WOF5] ermittelt. Die Verbindung kristallisiert tetragonal in der Raumgruppe I4 mit zwei Formeleinheiten pro Elementarzelle (975 unabhängige Reflexe, R = 0,052). Das [WOF5]⊖-Anion befindet sind auf einer Lage mit Punktsymmetrie 4; es ist somit fehlgeordnet. Die Verfeinerungsrechnung eines Strukturmodells unter Verwendung von split-Positionen läßt einen deutlichen π-Bindungsanteil der WO-Bindung erkennen, der zum Abdrängen der äquatorialen F-Atome aus der Ebene mit dem Wolframatom führt (  OWFeq. = 96,4°).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19824930105
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    Kristallstruktur und spektroskopische Daten von Rb2[VOF4(H2O)] (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 506 (1983), S. 169-177 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure and Spectroscopic Data of Rb2[VOF4(H2O)]Blue crystals of Rb2[VOF4(H2O)] have been obtained from hydrofluoric acid. The crystal structure (space group Cmcm, a = 969.6(4), b = 780.6(2), c = 835.4(4) pm, Z = 4, dc = 3.486 gcm-3, dm = 3.41 gcm-3, Rw = 0.032 for 411 independent reflections) shows isolated [VOF4(H2O)]2- anions  -  with H2O in trans-position to the relatively long V—O bond (d(V—O) = 166.8(7) pm)  -  which are connected with each other by hydrogen bonds forming infinite chains. The blue colour of the compound despite of the isotypism to the “green” modification of Cs2[VOF4(H2O)] is discussed on the basis of the structural data, i.r./Raman and u.v./vis reflection spectra. The magnetic moment is 1.72 B.M. at 295 K.
    Notes: Blaue Kristalle von Rb2[VOF4(H2O)] wurden aus flußsaurer Lösung erhalten. Ihre Kristallstruktur (Raumgruppe Cmcm, a = 969,6(4), b = 780,6(2), c = 835,4(4) pm, Z = 4, dc = 3,486 gcm-3, dm = 3,41 gcm-3, Rw = 0,032 für 411 unabhängige Reflexe) weist isolierte [VOF4(H2O)]2--Anionen auf mit H2O in trans-Stellung zur relativ langen V—O-Bindung (d(V—O) = 166,8(7) pm), die über Wasserstoffbrückenbindungen zu unendlichen Ketten miteinander verknüpft sind. Die trotz Isotypie mit der „grünen“ Modifikation von Cs2[VOF4(H2O)] blaue Farbe wird auf der Basis der Strukturdaten sowie der IR/Raman- und UV/VIS-Reflexionsspektren diskutiert. Das magnetische Moment beträgt bei 295 K 1,72 B.M.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19835061120
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