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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: Cobalt(II) complex ; 1,2-dimethyl-5-nitro-imidazole ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Crystal Structure of Bis(1,2-dimetyl-5-nitro-imidazole)dichlorocobalt(II)Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II) was obtained by reaction of CoCl2 · 6 H2O with 1,2-dimethyl-5-nitro-imidazole in methanol. The compound forms blue crystals which were characterized by IR and UV-vis spectroscopy and by an X-ray crystal structure determination. Co(C5H7N3O2)2Cl2: tetragonal, space group I42d, Z = 8, a = 1142.1(1) pm, c = 2577.3(2) pm. R = 0.036 for 670 independent reflexions. The Co atom is tetrahedrally surrounded by two chlorine and two N atoms at distances of 222.8(2) and 203.5(4) pm.
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  • 3
    ISSN: 0044-2313
    Keywords: Trinuclear zirconium complex ; phosphanido ligand ; phosphinidene ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P—H-functionalised Phosphanido Ligands in Transition Metal Chemistry: Molecular Structure of CpZr(μ-PHtBu)2(μ-PtBu)2 {Zr(μ-Cl)Cp}2The reaction of polymeric [CpZrCl3]n with solvent-free LiPHtBu yields the trinuclear ZrIII/ZrIV complex CpZr(μ-PHtBu)2(μ-PtBu)2 {Zr(μ-Cl)Cp}2 (1) in a redox reaction in low yield. The oxidation product (PHtBu)2 is observed by 31P-NMR spectroscopy. 1 crystallises tetragonal in the space group P43212 with a = 1130.5(5) pm and c = 3415.7(5) pm.
    Notes: Die Reaktion von polymerem [CpZrCl3]n mit solvatfreiem LiPHtBu liefert in einer Redoxreaktion den dreikernigen ZrIII/ZrIV-Komplex CpZr(μ-PHtBu)2(μ-PtBu)2{Zr(μ-Cl)Cp}2 (1) in geringer Ausbeute. 31P-NMR-spektroskopisch kann die Bildung des Oxidationsprodukts (PHtBu)2 gezeigt werden. 1 kristallisiert tetragonal in der Raumgruppe P43212 mit a = 1130,5(5) pm und c = 3415,7(5) pm.
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  • 4
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium heptathiacyclo thioarsenate(III) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenylphosphonium Heptathiacyclo Thioarsenate(III), PPh4[SAsS7]From PPh4[As2SCl5] und K2S5 the title compound was obtained in acetonitrile among other products. According to an X-ray crystal structure analysis, it crystallizes in the orthorhombic space group Pna21 with a = 1 826.1(3), b = 1 312.0(2), c = 1 215.9(2) pm, Z = 4. The structure consists of PPh4+ and [SAsS7]- ions, AsS7 rings in the crown conformation as in S8 being present.
    Notes: Aus PPh4[As2SCl5] und K2S5 wurde in Acetonitril unter anderem die Titelverbindung erhalten. Nach der Röntgenstrukturanalyse mit 1474 beobachteten Reflexen (R = 7,1%, wR = 2,7%) kristallisiert sie rhombisch in der Raumgruppe Pna21; a = 1 826,1(3), b = 1 312,0(2), c = 1 215,9(2) pm, Z = 4. Die Struktur besteht aus PPh4+-und [SasS7]-Ionen, wobei AsS7-Ringe in der Kronenform wie beim S8 vorliegen.
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  • 5
    ISSN: 0044-2313
    Keywords: 2,2′-Bipyridyl molybdenum difluoridedioxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of [MoO2F2(2,2′-bipyridyl)]The title compound crystallizes in the space group P21/n with a = 869.6(1), b = 1390.1(3), c = 959.0(1) pm, β = 110.967(5)°, Z = 4; structure determination with 1718 observed independent reflections, R = 0.031. The compound consists of molecules having two cis oxo ligands and a bipyridyl chelate in the MoO2 plane.
    Notes: Die Titelverbindung kristallisiert in der Raumgruppe P21/n mit a = 869,6(1); b = 1390,1(3); c = 959,0(1) pm; β = 110,967(5)°, Z = 4; Strukturbestimmung mit 1718 beobachteten unabhängigen Reflexen, R = 3,1%. Die Verbindung besitzt eine Molekülstruktur mit cis-ständigen Oxoliganden und dem Bipyridylchelat in der MoO2-Ebene.
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  • 6
    ISSN: 0044-2313
    Keywords: Rhenium tetrachloride chelate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Complexes of Rhenium Tetrachloride. The Crystal Structures of ReCl4(DME) and ReCl4(DPPE) · TolanBright green crystals of ReCl4(DME) have been prepared by the reaction of rhenium pentachloride with dimethoxyethane (DME) in dichloromethane. ReCl4(DPPE) · tolan was obtained in form of red crystals by the reaction of the alkyne complex [ReCl4(Ph—C≡C—Ph)(POCl3)] with bis(diphenylphosphino)ethane (DPPE) in dichloromethane. The complexes were characterized by X-ray structure determinations.ReCl4(DME): Space group I42d, Z = 8, 829 observed unique reflexions, R = 0.022. Lattice dimensions at 19.5°C: a = b = 960.60(6), c = 2337.2(6) pm. The complex forms monomeric molecules with DME as chelating ligand; the Re—O bond lengths are 213.1 pm. The chlorine atoms, arranged in trans position to the chelating ligand, have slightly shorter Re—Cl bonds than the chlorine atoms in cis position (232,1 pm).ReCl4(DPPE) · tolan: Space group P21/n, Z = 4,4313 observed unique reflexions, R = 0.040. Lattice dimensions at -80°C: a = 1095.7(1), b = 1764.2(2), c = 1898.0(2) pm, β = 99.229(8)°. The compound consists in form of monomeric molecules [ReCl4(DPPE)] and diphenylacetylene molecules, which are incorporated in the lattice. The two phenyl rings of the tolan molecules are twisted towards each other along the C—C axis with a dihedral angle of 21°. The DPPE molecules are bonded to the rhenium atom in a chelating fashion with medium Re—P lengths of 250.4 pm. The chlorine atoms, arranged in trans position to this ligand, with Re—Cl bond lengths of 234.5 pm are slightly longer than the Re—Cl bonds in cis position with 232.3 pm.
    Notes: ReCl4(DME) wird in Form leuchtend grüner Kristalle durch Reaktion von Rheniumpentachlorid mit Dimethoxyethan (DME) in Dichlormethan hergestellt. ReCl4(DPPE) · Tolan erhielten wir als rote Kristalle bei der Reaktion des Alkinkomplexes [ReCl4(Ph—C≡C—Ph)(POCl3)] mit Bis(diphenylphosphino)ethan (DPPE) in Dichlormethan. Die Komplexe wurden durch röntgenographische Strukturanalysen charakterisiert.ReCl4(DME): Raumgruppe I42d, Z = 8, 829 beobachtete unabhängige Reflexe, R = 2,2%. Gitterkonstanten bei 19,5°C: a = b = 960,60(6); c = 2337,2(6) pm. Der Komplex bildet monomere Moleküle mit dem DME-Liganden als Chelat und Re—O-Abständen von 213,1 pm. Die hierzu trans-ständig angeordneten Chloratome haben mit 228,1 pm etwas kürzere Re—Cl-Bindungen als die cis-ständigen Cl-Atome (232,1 pm).ReCl4(DPPE) · Tolan: Raumgruppe P21/n, Z = 4, 4313 beobachtete, unabhängige Reflexe, R = 4,0%. Gitterkonstanten bei -80°C: a = 1095,7(1); b = 1764,2(2); c = 1898,0(2) pm, β = 99,229(8)°. Der Komplex bildet monomere Moleküle [ReCl4(DPPE)] und in das Gitter eingelagerte Diphenylacetylenmoleküle, deren Phenylringe einen Diederwinkel von 21° zueinander bilden. Die DPPE-Moleküle sind chelatartig am Rheniumatom gebunden mit Abständen Re—P von im Mittel 250,4 pm. Die hierzu trans-ständig angeordneten Chloratome sind mit Re—Cl—Abständen von 234,5 pm etwas länger als die cis-ständigen Re—Cl-Bindungen mit 232,3 pm.
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  • 7
    ISSN: 0044-2313
    Keywords: Rubidium vanadate (IV, V) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Access to Alkali Vanadates(IV,V) Crystal Structure of Rb2V3O8By heating vanadium(V) oxide with rubidium iodide to 500°C, the vanadium experiences partial reduction and Rb2V3O8 is obtained. It has the fresnoite structure. Crystal data: a = 892.29(7), c = 554.49(9) pm at 20°C, tetragonal, space group P4bm, Z = 2. X-ray crystal structure determination with 620 observed reflexions, R = 0.027. V2O7 units share vertices with VO5 square pyramids, forming layers; a layer can be regarded as association product of VO2+ and V2O74- ions. The Rb+ ions between the layers have pentagonal-antiprismatic coordination.
    Notes: Beim Erhitzen von Vanadium(V)-oxid mit Rubidiumiodid auf ca. 500°C wird Vanadium partiell reduziert, es entsteht Rb2V3O8. Dieses kristallisiert in der Fresnoit-Struktur. Kristalldaten: a = 892,29(7), c = 554,49(9) pm bei 20°C, tetragonal, Raumgruppe P4bm, Z = 2. Röntgenstrukturbestimmung mit 620 beobachteten Reflexen, R = 2,7%. V2O7-Einheiten und quadratische Pyramiden VO5 sind untereinander zu Schichten eckenverknüpft; die Schicht kann als Assoziat aus VO2+ - und V2O74--Ionen aufgefaßt werden. Die Rb+-Ionen zwischen den Schichten sind verzerrt pentagonal-antiprismatisch koordiniert.
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  • 8
    ISSN: 0044-2313
    Keywords: Indium polysulfido complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of (PPh4)2[In(S4)(S6)Cl] and (PPh4)2[In(S4)Cl3]InCl and PPh4Cl yield (PPh4)2[In2Cl6] in acetonitrile. This reacts with Na2S4 in presence of PPh4Cl, forming (PPh4)2[In(S4)(S6)Cl]. Its crystal structure was determined by X-ray diffraction (R = 0.075, 2 282 observed reflexions). It is isotypic with (PPh4)2[In(S4)(S6)Br] and contains anions with trigonal-bipyramidal coordination of In, Cl occupying an axial position, and the S4 and S6 groups being bonded in a chelate manner. The reaction of (PPh4)2[In2Cl6] and sulfur in acetonitrile yielded (PPh4)2[InCl5] and (PPh4)2[In(S4)Cl3]. The crystal structure analysis of the latter (R = 0.072, 4 080 reflexions) revealed an anion with distorted trigonal-bipyramidal coordination of In, the S4 group occupying one axial and one equatorial position; the S4 group shows positional disorder.
    Notes: Aus InCl und PPh4Cl entsteht in Acetonitril (PPh4)2[In2Cl6]. Aus diesem wurde mit Na2S4 im Beisein von PPh4Cl (PPh4)2[In(S4)(S6)Cl] erhalten. Seine Kristallstruktur wurde mittels Röntgenbeugung bestimmt (R = 7,5%, 2 282 beobachtete Reflexe). Es kristallisiert isotyp zum (PPh4)2[In(S4)(S6)Br] und enthält Anionen mit trigonal-bipyramidaler Koordination des In; das Cl-Atom nimmt eine axiale Position ein und die S4- und S6-Gruppe ist jeweils chelatartig gebunden. Aus (PPh4)2[In2Cl6], PPh4Cl und Schwefel entstanden in Acetonitril (PPh4)2[InCl5] und (PPh4)2[In(S4)Cl3]. Nach der Kristallstruktur des letzteren (R = 7,2%, 4 080 Reflexe) ist im [In(S4)Cl3]2--Ion das In-Atom verzerrt trigonal-bipyramidal koordiniert, wobei die S4-Gruppe an eine axiale und eine equatoriale Position gebunden ist; die S4-Gruppe ist fehlgeordnet.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1033-1034 
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium-tetradecachlorotetraarsenate(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraphenylphosphonium Tetradecachlorotetraarsenate(III), (PPh4)2As4Cl14The title compound was obtained by reaction of As4S4, PPh4Cl and chlorine in dichloromethane. According to its X-ray crystal structure analysis, the As4Cl142- ion can be described as an association product of two AsCl4- units and two AsCl3 molecules. The As atoms and ten Cl atoms are approximately in a plane, the remaining four Cl atoms alternately take positions above and below this plane. The As atoms have distorted ψ octahedral coordination.
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  • 10
    ISSN: 0044-2313
    Keywords: Tungsten bronze, Cs0.29WO3 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A Novel Synthetic Access to the Tungsten Bronze Cs0.29WO3 and its Crystal StructureThe hexagonal tungsten bronze Cs0.29WO3 was obtained in form of black, prismatic crystal by the reduction of WO3 with molten cesium iodide at 700°C. Its crystal structure was determined by X-ray diffraction (399 unique observed reflexions, R = 0.058). Crystal data: a = 741.2(3), c = 760.0(5) pm, space group P6322, Z = 6. It corresponds to the known structure of hexagonal tungsten bronzes, having tungsten atoms displaced from the octahedra centres by 11.9 pm and with three different W—O bond lengths (198, 191, 187 pm). The WO6 octahedra are slightly titled mutually.
    Notes: Bei der Reaktion von WO3 in einer Caesiumiodid-Schmelze bei 700°C entsteht die hexagonale Wolframbronze Cs0.29WO3 in Form schwarzer, hexagonal-prismatischer Kristalle. Ihre Struktur wurde durch Röntgenbeugung bestimmt (399 beobachtete unabhängige Reflexe, R = 5,8%). Kristalldaten: a = 741,2(3), c = 760,0(5) pm, Raumgruppe P6322, Z = 6. Es handelt sich um die bekannte Struktur der hexagonalen Wolframbronzen mit Wolframatomen, die aus den Oktaedermitten um 11,9 pm herausgerückt sind und mit drei verschiedenen W—O-Bindungslängen (198, 191, 187 pm). Die WO6-Oktaeder sind leicht gegeneinander verkippt.
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