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  • crystal structures  (8)
  • Organic Chemistry  (3)
  • 2,2′-Bipyridyl molybdenum difluoridedioxide  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Bildung, Kristallstruktur und absolute Konfiguration von (-)-N-(Chloromethyl)galanthaminium-chlorid (1994)
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 77 (1994), S. 1611-1615 
    Details
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Formation, X-Ray Crystal Structure, and Absolute Configuration of (-)-N-(Chloromethyl)galanthaminium ChlorideThe acetylcholinesterase inhibitor galanthamine (1), main alkaloid of several Narcissus species, readily forms a quaternary ammonium salt by reaction with the solvent CH2Cl2. The structure and absolute configuration of (-)-N-(chloromethyl)galanthaminium chloride (2) were determined by X-ray diffraction (R = 0.075 for 2775 observed independent reflexions) and NMR spectroscopy. The tetragonal crystals (space group P43) contain two crystallographically independent cations which do not differ significantly from one another. The CH2Cl group is attached to the quaternary N-atom in stereospecific (R)-configuration. In the crystal, the configurational position of the Me group at the N-atom of 2 differs from that of the crystalline free base 1. Hydrogen bonding is observed from the OH group at C(3) of 2 to the Cl- anion or to the Cl-atom of an adjacent cation.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/hlca.19940770617
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  • 2
    Electronic Resource
    Electronic Resource
    Intramolekulare Addition von Carbanionen an Anthrachinone (1984)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 1984 (1984), S. 306-318 
    Details
    ISSN: 0170-2041
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Intramoleclar Addition of Carbanions to AnthraquinonesThe intramolecular Michael addition of the carbanions derived from the β-keto diesters 15a and 15b yields the naphthacenequinones 20a and 20b. In contrast, the similar dimethyl ether 11 cyclizes to give the benzo[α]anthracenequinone 17. The hydroquinone of 1,8-dihydroxyanthraquinone (5a) reacts with acrylate to yield the unusual anthrone derivatives 12b and 12c.
    Notes: Die intramolekulare Michael-Addition der Carbanionen, die sich von den β-Ketodiestern 15a und 15b ableiten, liefert die Naphthacenchinone 20a und 20b. Dagegen cyclisiert der Dimethylether 11 zum Benzo[α]anthracenchinon 17. Das Hydrochinon des 1,8-Dihydroxyanthrachinons (5a) reagiert mit Acrylsäureester zu den ungewöhnlichen Anthron-Derivaten 12b und 12c.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.198419840213
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  • 3
    Electronic Resource
    Electronic Resource
    über die Bildung einer Rubazonsäure aus Phenylhydrazinderivaten der Zucker (1961)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 648 (1961), S. 96-113 
    Details
    ISSN: 0075-4617
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Die Einwirkung von Perjodat auf Dextran, Xylan, Inulin und Saccharose führt zu Oxydationsprodukten dieser Zucker, die mit Phenylhydrazin unter anderem Abkömmlinge der Rubazonsäure ergeben.  -  Die gleichen Verbindungen entstehen bei Einwirkung von asymmetrisch disubstituierten Arylhydrazinen auf D-Fructoson-1-phenylhydrazon oder auf Glycerose-phenylosazon und durch Umsetzung von Glycerinaldehyd-methylphenylhydrazon mit Phenylhydrazin. Es wird über Synthese und Eigenschaften dieser Verbindungen berichtet.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jlac.19616480114
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  • 4
    Electronic Resource
    Electronic Resource
    Neue Synthesewege für Thiohalogeno- und Cyclothioarsenate(III). Kristallstrukturen von PPh4[As2SBr6] · CH3CN und PPh4[SAsS5] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 82-88 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium thiohalogenoarsenate(III) ; pentathiacyclothioarsenate(III) ; synthesis ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Novel Routes to the Synthesis of Thiohalogeno- and Cyclothioarsenates(III). Crystal Structures of PPh4[As2SBr6] · CH3CN and PPh4[SAsS5]By reactions of (PPh4)2[As2Cl8] and (PPh4)2[As2Br8] with Na2S4 in acetonitrile (PPh4)2[As2SCl6] · CH3CN and (PPh4)2[As2SBr6] · CH3CN were obtained, respectively. Using K2S5, PPh4[As2SCl5] and PPh4[SAsS5] were the products. The latter can also be obtained from PPh4[As2SCl5] and Na2S4, while PPh4[As3S3Br4] is formed from PPh4[As2SBr5] with K2S5. Two X-ray crystal structure determinations were performed. PPh4[As2SBr6] · CH3CN: triclinic, P1, Z = 2, a = 1200.4(7), b = 1507.3(6), c = 1594.4(8) pm, α = 81.59(2), β = 78.22(3), γ = 80.58(2)°, R = 0.096 for 2298 observed reflexions. The structure contains [As2SBr6]2- -ions in which the two Sb atoms are joined via one S and two Br atoms. PPh4[SAsS5]: triclinic, P1, Z = 2, a = 1133.9(4), b = 1142.5(4), c = 1186.9(5) pm, α = 102.77(4), β = 107.74(3), γ = 106.65(3)°, R = 0.043 für 2677 reflexions. In the [SAsS5]- -ion an AsS5 ring in the chair conformation is present.
    Notes: Durch Reaktionen von (PPh4)2[As2Cl8] und (PPh4)2[As2Br8] mit Na2S4 in Acetonitril wurden (PPh4)2[As2SCl6] · CH3CN bzw. (PPh4)2[As2SBr6] · CH3CN hergestellt. Mit K2S5 entstanden PPh4[As2SCl5] bzw. PPh4[SAsS5]. Letzteres ist auch aus PPh4[As2SCl5] und Na2S4 zugänglich, während PPh4[As3S3Br4] aus PPh4[As2SBr5] mit K2S5 entsteht. Zwei Kristallstrukturen wurden durch Röntgenbeugung bestimmt.PPh4[As2SBr6] · CH3CN: triklin, P1, Z = 2, a = 1200,4(7), b = 1507,3(6), c = 1594,4(8) pm, α = 81,59(2), β = 78,22(3), γ = 80,58(2)°. R = 9,6% für 2298 beobachtete Reflexe. Die Struktur enthält [As2SBr6]2- - Ionen, in denen die beiden Sb-Atome über ein S- und zwei Br-Atome miteinander verbunden sind. PPh4[SAsS5]: triklin, P1, Z = 2, a = 1133,9(4), b = 1142,5(4), c = 1186,9(5) pm, α = 102,77(4), β = 107,74(3), γ = 106,65(3)°, R = 4,3% für 2677 Reflexe. Im [SAsS5]- -Ion ist ein AsS5-Ring in Sesselkonformation vorhanden.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090316
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  • 5
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Thiochloroantimonate(III) PPh4[Sb2SCl5] und (PPh4)2[Sb2SCl6] · CH3CN (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 89-94 
    Details
    ISSN: 0044-2313
    Keywords: Thiopentachlorodiantimonate(III) ; thiohexachlorodiantimonate(III) ; 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 Thiochloroantimonates(III) PPh4[Sb2SCl5] and (PPh4)2[Sb2SCl6]. CH3CN(PPh4)2Sb3Cl11, obtained from Sb2S3, PPh4Cl and HCl, reacts with Na2S4 in acetonitrile forming PPh4[Sb2SCl5]. From this and Na2S4 or from (PPh4)2[Sb2Cl8] and Na2S4 or K2S5 in acetonitrile (PPh4)2[Sb2SCl6] · CH3CN is obtained. Data obtained from the X-ray crystal structure determinations are: PPh4[Sb2SCl5], monoclinic, space group P21/c, a = 1002.9(3), b = 1705.6(5), c = 1653.7(5) pm, β = 99.12(2)°, Z = 4, R = 0.068 for 1283 reflextions; (PPh4)2[Sb2SCl6] · CH3CN, triclinic, space group P1, a = 1287.8(7), b = 1343.6(9), c = 1696.5(9) pm, α = 69.82(5), β = 85.08(4), γ = 71.54(6)°, Z = 2, R = 0.059 for 6409 reflexions. In every anion two Sb atoms are linked via one sulfur and one ore two chloro atoms, respectively. Paris of [SbSCl5]- ions are associated via Sb … S and Sb … Cl contacts forming dimer units. In both compounds every Sb atom has a distorted octahedral coordination when the lone electron pair is included in the counting.
    Notes: (PPh4)2Sb3Cl11, das aus Sb2S3, PPh4Cl und HCl erhalten wurden, reagiert mit Na2S4 in Acetonitril unter Bildung von PPh4[Sb2SCl5]. Aus diesem und Na2S4 oder aus (PPh4)2[Sb2Cl8] und Na2S4 oder K2S5 wird in Acetonitril (PPh4)2[Sb2SCl6] · CH3CN erhalten. Die Kristallstrukturbestimmungen mit Hilfe der Röntgenbeugung ergaben: PPh4[sb2SCl5], monoklin, Raumgruppe P21/c, a = 1002,9(3), b = 1705,6(5), c = 1653,7(5) pm, β = 99,12(2)°, Z = 4, R = 6,8% für 1283 Reflexe; (PPh4)2[Sb2SCl6] · CH3CN, triklin, Raumgruppe P1, a = 1287,8(7), b = 1343,6(9), c = 1696,5(9) pm, α = 69,82(5), β = 85,08(4), γ = 71,52(6)°, Z = 2, R = 5,9% für 6409 Reflexe. In den Anionen sind jeweils zwei Sb-Atome vorhanden, die über ein S- und ein bzw. zwei Cl-Atome miteinander verknüpft sind. Paare von [Sb2SCl5]- -Ionen sind über vier Sb … S und Sb … Cl-Kontakte miteinander zu einer dimeren Einheit assoziiert. In beiden Verbindungen hat ein Sb-Atom eine verzerrt oktaedrische Koordination, wenn man das einsame Elektronenpaar mitzählt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090317
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  • 6
    Electronic Resource
    Electronic Resource
    η-Mo4O11 und Mg2Mo3O8: eine neue Synthese und Verfeinerung ihrer Kristallstrukturen (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 541-545 
    Details
    ISSN: 0044-2313
    Keywords: Dimagnesium trimolybdate(IV) ; molybdenum oxide ; preparation ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: η-Mo4O11 and Mg2Mo3O8: a New Way of Synthesis and Refinement of their Crystal StructuresMg2Mo3O8 was obtained by solid state reaction of MgI2 and MoO3 (1:1) at 200°C and subsequent crystallization at 800°C. Under the same conditions, ZnI2 and MoO3 only yielded rather impure Zn2Mo3O8; however, when ZnI2 or CdI2 and MoO3 were taken in a molar ratio of 1:2, well crystallized η-Mo4O11 was obtained. The known crystal structures of Mg2Mo3O8 and η-Mo4O11 were refined with new X-ray diffraction data (R = 0.030 and 0.059, respectively). The kind of twinning of monoclinic η-Mo4O11 is discussed.
    Notes: Durch Festkörperreaktion von MgI2 und MoO3 (1:1) bei 200°C und anschließender Kristallisation bei 800°C entsteht Mg2Mo3O8. Mit ZnI2 entsteht unter den gleichen Bedingungen nur stark verunreinigtes Zn2Mo3O8; beim Einsetzen von ZnI2 oder CdI2 und MoO3 im Molverhältnis von 1:2 wird dagegen gut kristallisiertes η-Mo4O11 erhalten. Die bekannten Kristallstrukturen von Mg3Mo8O8 und η-Mo4O11 wurden mit neuen Meßdaten verfeinert (R = 3,0 bzw. 5,9%). Die Art der Zwillingsbildung des monoklinen η-Mo4O11 wird diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210407
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  • 7
    Electronic Resource
    Electronic Resource
    Die Bildung von PPh4[WOCl4 · THF] und PPh4Cl · 4As4S3 aus W(CO)6 und PPh4[As2SCl5] sowie ihre Kristallstrukturen (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 77-81 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium pentachlorothioarsenate(III) ; tetraphenylphosphonium tetrachlorooxotungstate; ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of PPh4[WOCl4 · THF] and PPh4Cl · 4As4S3 from W(CO)6 and PPh4[As2SCl5] and their Crystal StructuresWhen W(CO)6 and PPh4[As2SCl5] are irradiated with UV light in tetrahydrofurane, PPh4[WOCl4 · THF], PPh4 Cl· 4As4S3 and PPh4[Cl2H] are obtained. X-ray crystal structure determinations were performed. PPh4[WOCl4 · THF], monoclinic, space group P21/c, Z = 4, a = 1207.5(2), b = 1003.7(2), c = 2642.0(5) pm, β = 114.71(1)°, R = 0.049% for 2824 reflexions; PPh4+ and [WOCl4. THF]- ions are present, the WOCl4 group having the shape of a tetragonal Pyramid with a short W = O bond (169 pm) and the THF molecule being weakly associated (W—O 236 pm). PPh4Cl · 4AsS3, tetragonal, I41/a, Z = 4, a = 1742.3(3), c = 1664.5(4) pm, R = 0.066% for 1350 reflexions; it consists of separate PPh4+ and Cl- ions and As4S3 molecules.
    Notes: Bei der Bestrahlung von W(CO)6 und PPh4[As2SCl5] mit UV-Licht in Tetrahydrofuran entstehen PPh4[WOCl4 · THF], PPh4Cl · 4As4S3 und PPh4[Cl2H]. Von den beiden ersteren wurden die Kristallstrukturen mittels Röntgenbeugung aufgeklärt. PPh4[WOCl4 · THF]: monoklin, Raumgruppen P21/c, Z = 4, a = 1207,5(2), b = 1003,7(2), c = 2642,0(5) pm, β = 114,71(1)°, R = 4,9% für 2824 Reflexe; es ist aus Ionen PPh4+ und [WOCl4 · THF]- aufgebaut, wobei die WOCL4-Gruppe die Gestalt einer quadratischen Pyramide mit einem kurzen W = O-Abstand (169 pm) hat und das THF-Molekül relativ locker daran assoziiert ist (W—O 236 pm). PPh4Cl · 4As4S3: tetragonal, I41/a, Z = 4, a = 1742,3(3), c = 1664,5(4) pm, R = 6,6% für 1350 Reflexe; es besteht aus einzelnen Ionen PPh4+ und Cl- sowie As4S3-Molekülen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090315
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  • 8
    Electronic Resource
    Electronic Resource
    Die Kristallstruktur von [MoO2F2(2,2′-Bipyridyl)] (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 117-120 
    Details
    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.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926100119
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  • 9
    Electronic Resource
    Electronic Resource
    Synthese und Kristallstrukturen der Polyselenidokomplexe (PPh4)6[M(Se4)2]2[WSe4] · DMF mit M = Zink und QuecksilberHerrn Prof. Dr. Erhard Uhlemann zum 60. Geburtstage gewidmet (1992)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 12-18 
    Details
    ISSN: 0044-2313
    Keywords: Mixed polyselenido complexes of zinc/tungsten, Mercury/tungsten ; crystal structures ; FIR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Polyselenido Complexes (PPh4)6[M(Se4)2]2[WSe4] · DMF with M = Zinc and MercuryThe title compounds have been prepared by the reactions of the acetates of zinc and mercury, respectively, with excess (PPh4)2 WSe4 in boiling dimethylformamide, forming black-red single crystals. According to the X-ray structure determinations both compounds crystallize isotypically in the space group 12/a with four formula units per unit cell. (PPh4)6[Zn(Se4)2]2[WSe4] · DMF: a = 2888.1(6), b = 1740.3(2), c = 2893.9(4) pm, β = 90.47(1)°. 3230 observed unique reflections, R = 0.009.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891.8(5), b = 1738.0(4), c = 2920.1(5) pm, β = 90.29(2)°. 2978 observed unique reflections, R = 0.115%.The compounds consist of PPh4+ ions, spirocyclic octaseleno metallates [M(Se4)2]2-, tetrahedral WSe42-ions, and disordered DMF Molecules.
    Notes: Die Titelverbindungen entstehen in Form schwarz-roter Einkristalle beim Erhitzen der Acetate von Zink und Quecksilber mit überschüssigem (PPh4)2 WSe4 in Dimethylformamid-Lösungen. Nach den Röntgenstrukturanalysen kristallisieren die Verbindungen isotyp in der Raumgruppe I2/a mit vier Formeleinheiten pro Elementarzelle. (PPh4)6[Zn(Se4)2]2[WSe4]· DMF: a = 2888,1(6), b = 1740,3(2), c = 2893,9(4) pm, β = 90,47(1)°. 3230 beobachtete unabhängige Reflexe, R = 9,9%.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891,8(5), b = 1738,0(4), c = 2920,1(5) pm, β = 90,29(2)°. 2978 beobachtete unabhängige Reflexe, R = 11,5%.Die Verbindungen bestehen aus PPh4 +-Ionen, spirocyclischen Octaselenometallaten [M(Se4)2]2-, tetraedrischen WSe42- Ionen und eingelagerten, fehlgeordneten DMf-Molekülen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19926090303
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  • 10
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    Electronic Resource
    Synthese und Kristallstrukturen von (PPh4)2[As2Se4Cl12] und (PPh4)2[As2Se4Br12]Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 790-794 
    Details
    ISSN: 0044-2313
    Keywords: Diselenium dihalide complexes ; arsenic trihalide and halide ions ; crystal structures ; 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[As2Se4Cl12] and (PPh4)2[As2Se4Br12]The reaction of PPh4Cl and As2Se3 with SOCl2 or with chlorine in dichloromethane affords (PPh4)2[As2Se4Cl12] with good yields. From PPh4Br, As2Se3 and bromine the corresponding bromo compound was obtained. According to the X-ray crystal structure determinations both compounds are isotypic, crystallizing in the space group of P1. In the anions two Se2X2 molecules are linked with two X- ions forming an Se4X2 ring in chair conformation. Each X--ion is associated with an additional AsX3 molecule (X = Cl, Br).
    Notes: Bei der Umsetzung von PPh4Cl und As2Se3 mit SOCl2 oder mit Chlor in Dichlormethan entsteht (PPh4)2[As2Se4Cl12] in guter Ausbeute. Aus PPh4Br, As2Se3 und Brom entsteht die entsprechende Bromoverbindung. Nach den Röntgenstrukturanalysen kristallisieren beide Verbindungen isotyp in der Raumgruppe P1. Die Anionen können als Assoziate aus je zwei Se2X2-Molekülen und zwei X--Ionen aufgefaßt werden, unter Ausbildung eines Se4X2-Sesselringes; an jedes X--Ion ist noch ein AsX3-Molekül angelagert (X = Cl, Br).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220507
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