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  • 1
    ISSN: 0044-2313
    Keywords: Bis(1, 3-diketonato)cobalt-bisimidazoles ; crystal structure ; thermal degradation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Thermal Degradation of Bis(1,3-diketonato)cobaltbisimidazolesThe crystal structure of Co(bzac)2(HIm)2. 2MeOH (I) and Co(acac)2(HIm)2 (II) were determined by x-ray diffraction. II: triclinic, space group P1, Z = 2, a = 746.3(1), b = 948.2(1), c = 1396.7(2)pm, α = 85.18(1)°, β = 88.96(1)°, γ = 80.72(1)°, R = 3.0% for a total of 2194 observed reflections. I: monoclinic, P21/c, Z = 2, a = 964.2(3), b = 864.5(2), c = 1769.8(4)pm, β = 98.87(2)°, R = 4.7% for a total of 967 observed reflections. In both compounds centrosymmetric molecules with two bidentate diketonato groups and two imidazole ligands in trans-position are present. The molecules of II are linked by N—H…O-bridges within layers, while in the lattice of I by the interaction with methanol molecules N-H…O-H…O-bridges are formed.The nature of the H-bridges is the deciding factor for the first step of the thermal degradation of the complexes. The N-H…O-bridges of II relieves the change of the acidic protons of the imidazole to the acetylacetonato ligands. Therefore in the first step acetylacetone is eliminated. No such bridges are present in the complex I. Therefore, in the first step, imidazole and methanol are removed. On heating in O-donor solvents the reaction of I is quite analogous, and this is the reason for the application of this complex as a latent initiator of the epoxide polymerisation.
    Notes: Die Kristallstrukturen von Co(bzac)2(HIm)2 · 2MeOH (I) und Co(acac)2(HIm)2 (II) wurden durch Röntgenbeugung bestimmt. II: triklin, Raumgruppe P1, Z = 2, a = 746,3(1), b = 948,2(1) c = 1396,7(2)pm, α = 85,18(1)°, β = 88,96(1)°, γ = 80, 72(1)°, R = 3,0% fur 2194 beobachtete Reflexe; I: monoklin, P21/c, Z = 2, a = 964,2(3), b = 864,5(2), c = 1769,8(4)pm, β = 98,87(2)°, R = 4,7% für 967 Reflexe. In beiden Verbindungen liegen zentrosymmetrische Moleküle vor mit jeweils zwei chelatartig gebundenen Diketonatgruppen und zwei transständigen Imidazol-Liganden. Bei II sind die Moleküle über N—H…O-Brücken zu Schichten miteinander verknüpft, während bei I eine Verkettung über die Methanol-Moleküle mit N—H…O…H…O-Brücken vorliegt. Die Art der H-Brücken ist maßgebend für den ersten Schritt des thermischen Abbaus der Komplexe. Die N—H…O-Brücken von II erleichtern den Übergang der aciden Protonen der Imidazol- auf die Acetylacetonatoliganden. Im ersten Schritt wird daher Acetylaceton abgespalten. Dem Komplex I fehlen solche Brücken, deshalb werden im ersten Schritt Imidazol und Methanol eliminiert. Ganz analog verhält sich I beim Erhitzen in O-Donatorlösungsmitteln (Alkohole, Epoxide). I ist daher als latenter Initiator fur die Polymerisierung von Epoxiden geeignet.
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  • 2
    ISSN: 0044-2313
    Keywords: Osmium Polysulfido Complex ; Synthesis ; IR Spectrum ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Tetraphenylphosphonium Aqua-bis(tetrasulfido)thionitrosyl Osmate, PPh4[Os(NS)(S4)2(H2O)]PPh4[Os(NS)(S4)2(H2O)] has been prepared as redbrown crystals by reacting PPh4[OsNCl4] with a solution of excess disodium tetrasulfide in dimethylformamide/H2O and characterized by IR spectroscopy and by a crystal structure determination. Space group P21/n, Z = 4, structure solution with 4162 independent reflections, R = 0.059 for reflections with I 〉 2σ(I). Lattice dimensions at -40°C: a = 1138.9(5), b = 1301.4(4), c = 2092.7(7) pm, β = 104.74(3)º. Os—N, Os—O, and Os—S distances are 175.2(12), 219.8(12), and 237.5(4)-239.1(4) pm, respectively. The Os=N=S moiety is approximately linear, with an OsNS angle of 171.2(7)º.
    Notes: PPh4[Os(NS)(S4)2(H2O)] wurde als rotbraune Kristalle durch Reaktion von PPh4[OsNCl4] mit einer Lösung von überschüssigem Dinatriumtetrasulfid in Dimethylformamid/H2O hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/n, Z = 4, Strukturlösung mit 4162 unabhängigen Reflexen, R = 0,059 für Reflexe mit I 〉 2σ(I). Gitterabmessungen bei -40°C: a = 1138,9(5); b = 1301,4(4); c = 2092,7(7) pm, β = 104.74(3)º. Die Abstände Os—N, Os—O und Os—S betragen 175,2(12), 219,8(12) und 237,5(4) - 239,1(4) pm. Die Os=N=S-Gruppe ist mit einem Bindungswinkel von 171,2(7)º annähernd linear.
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  • 3
    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.
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  • 4
    ISSN: 0044-2313
    Keywords: Phosphorane Iminato Complexes of Titanium, Synthesis, Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphorane Iminato Complexes of Titanium. The Crystal Structures of [TiCl2(NPPh3)2] and [TiCl3(NPMe2Ph)(CH3CN)]2[TiCl2(NPPh3)2] has been prepared by the reaction of [TiCl3(NPPh3)] with excess Me3SiNPPh3 in a melt at 220°C, forming colourless crystals. [TiCl3(NPMe2Ph)(CH3CN)]2 is formed as yellow, moisture sensitive crystals from acetontrile solutions of [TiCl3(NPMe2Ph)]2, which on its part has been obtained by the reaction of TiCl4 with Me3SiNPMe2Ph. The complexes are characterized by IR spectroscopy and by crystal structure determinations.[TiCl2(NPPh3)2]. Space group Fdd2, Z = 8, structure refinement with 2875 observed unique reflections, R = 0.039. Lattice dimensions at 19°C: a = 2080.9, b = 3308.5, c = 973.6 pm. The compound forms monomeric molecules with bond lengths TiN of 179.0 pm and PN of 156.8 pm, which correspond with double bonds. The bond angle TiNP is 166.6°.[TiCl3(NPMe2Ph)(CH3CN)]2. Space group P1, Z = 1, structure refinement with 2577 unique reflections, R = 0.039 for reflections with I 〉 2σ(I). Lattice dimensions at 20°C: a = 856.6, b = 923.1, c = 1008.3 pm, α = 81.23°, β = 71.63°, γ = 81.41°. The compound forms centrosymmetric, dimeric molecules, in which the titanium atoms are linked via chloro bridges TiCl2Ti with TiCl bond lengths of 243.9 and 270.3 pm. In trans-position to the longer TiCl bonds the nitrogen atoms of the phosphorane iminato groups are coordinated with bond lengths TiN of 173.9 pm and PN of 161.4 pm which again correspond with double bonds. The bond angle TiNP is 156.4°.
    Notes: [TiCl2(NPPh3)2] wird in Form farbloser Kristalle durch Schmelzreaktion von [TiCl3(NPPh3)] mit überschüssigem Me3SiNPPh3 bei 220°C erhalten. [TiCl3(NPMe2Ph) · (CH3CN)]2 bildet gelbe, feuchtigkeitsempfindliche Kristalle, die aus Acetonitrillösung von [TiCl3(NPMe2Ph)]2 erhalten werden, welches seinerseits aus TiCl4 und Me3SiNPMe2Ph entsteht. Die Komplexe werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[TiCl2(NPPh3)2]. Raumgruppe Fdd2, Z = 8, Strukturverfeinerung mit 2875 beobachteten unabhängigen Reflexen, R = 0,039. Gitterabmessungen bei 19°C: a = 2080,9; b = 3308,5; c = 973,6 pm. Die Verbindung bildet monomere Moleküle mit Abständen TiN von 179,0 pm und PN von 156,8 pm, die Doppelbindungen entsprechen, und einem TiNP-Bindungswinkel von 166,6°.[TiCl3(NPMe2Ph)(CH3CN)]2. Raumgruppe P1, Z = 1, Strukturverfeinerung mit 2577 unabhängigen Reflexen, R = 0,039 für Reflexe mit I 〉 2σ(I). Gitterabmessungen bei 20°C: a = 856,6; b = 923,1; c = 1008,3 pm, α = 81,23°; β = 71,63°; γ = 81,41°. Die Verbindung bildet zentrosymmetrische, dimere Moleküle, in denen die Titanatome über TiCl2Ti-Brücken mit TiCl-Abständen von 243,9 und 270,3 pm verknüpft sind. In den trans-Positionen zu den langen Bindungen befinden sich die N-Atome der Phosphaniminatogruppen mit Abständen TiN von 173,9 pm und PN von 161,4 pm, die wiederum Doppelbindungen entsprechen. Der TiNP-Bindungswinkel beträgt 156,4°.
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  • 5
    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°.
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  • 6
    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.
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  • 7
    ISSN: 0022-328X
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
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  • 8
    ISSN: 0022-328X
    Keywords: Carbene ; Molybdenum ; Tungsten ; X-ray diffraction
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
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  • 9
    ISSN: 0022-328X
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 0022-328X
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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