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  • 1990-1994  (2)
  • 1975-1979  (3)
  • Inorganic Chemistry  (5)
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  • 1
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Bridges. I. Molecular and Crystal Structure of Phosphonic Acid H3PO3 - X-ray and Neutron Diffraction Studies of the Hydrogen and Deuterium CompoundsThe structure of phosphonic acid H3PO3 has been redetermined by single crystal neutron diffraction (λ = 104.22 pm) at 15.0 ± 0.1 K yielding lattice parameters {Pna21; Z = 8; a = 716.6(3); b = 1201.3(5); c = 674.3(3) pm} and bond lengths {mean values from two crystallographically independent molecules: P—O 155; P=O 150; P—H 139; O—H 101 pm} of high reliability (R = 0.053). Each molecule is involved in four asymmetric hydrogen bonds (O…H 155 to 160pm; O—H…O 168 to 177°) with either hydroxyl group donating and the phosphoryl fragment acting as a twofold acceptor. Thus a complex, three-dimensional net, consisting of four- and eight-point circuits in a 1:2 ratio, is put up although the molecules are packed in a comparatively simple way to form an almost cubic closest arrangement.An X-ray crystal structure determination (R = 0.032) carried out at 173 ± 3 K for comparison revealed no significant differences and angles between phosphorus and oxygen atoms; an additional comparing neutron diffraction study at 15.0 ± 0.1 K (λ = 131.68 pm; isotropic atomic displacement parameters) of the hydrogen (r = 0.044) and deuterium compounds (R = 0.041) resulted in nearly identical structural models for the two isotopomers.
    Notes: Die Struktur der Phosphonsäure H3PO3 wurde mittels Neutronenbeugung (λ = 104,22 pm) an einem Einkristall bei 15,0 ± 0,1 K neu bestimmt, so daß Gitterparameter {Pna21; Z = 8; a = 716,6(3); b = 1201,3(5); c 674,3(3) pm} und Bindungslängen {Mittelwerte aus zwei kristallographisch unabhängigen Molekülen: P—O 155; P = O 150; P—H 139; O—H 101 pm} nun sehr genau (R = 0,053) bekannt sind. Jedes Molekül nimmt teil an vier unsymmetrischen Wasserstoff-Brückenbindungen (O…H 155 bis 160 pm; O—H…O 168 bis 177°), wobei die Hydroxyl-Gruppen als Donoren und die Phosphoryl-Fragmente als jeweils zweifache Akzeptoren auftreten. Insgesamt wird so ein komplexes, aus Maschen von vier und acht Knoten im Verhältnis 1:2 bestehendes Raumnetz aufgespannt, obwohl die Moleküle selbst verhältnismäßig übersichtlich im Sinne einer kubisch dichtesten Anordnung gepackt sind.Eine zum Vergleich bei 173 ± 3 K durchgeführte Röntgenstrukturanalyse (R = 0,032) ergab in den P—O-Abständen und O—P—O-Winkeln kaum nennenswerte Unterschiede; eine zusätzliche, vergleichende Neutronenbeugungsuntersuchung bei 15,0 ± 0,1 K (λ = 131,68 pm; isotrope atomare Auslenkungsparameter) an der Hydrogen- (R = 0,044) und an der Deuterium-Verbindung (R = 0,041) führte zu weitgehend übereinstimmenden Strukturmodellen für die Isotopomeren.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 625-631 
    ISSN: 0044-2313
    Keywords: Bis(dichloromethyl)mercury ; Dichloromethylmercuryalkyles ; synthesis ; NMR, vibrational spectra ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Spectroscopic and X-Ray Structural Investigations on Dichloromethyl Mercury CompoundsBis(dichloromethyl)mercury, Hg(CHCl2)2, and mixed alkyl compounds RHgCHCl2 (with R = CH3, C2H5) have been synthesized by known methods from CH2Cl2, lithium butanide and HgCl2, CH3HgCl or C2H5HgCl, respectively. The 1H-, 13C-NMR as well as the IR and Raman spectra of the liquid alkyls RHgCHCl2 and the high melting Hg(CHCl2)2 have been measured and assigned. According to the X-ray structure determination Hg(CHCl2)2 crystallizes in the monoclinic space group P21/c with 4 non-symmetric molecules per unit cell (R = 0.046).
    Notes: Bis(dichlormethyl)quecksilber, Hg(CHCl2)2, und die gemischten Alkylverbindungen RHgCHCl2 (mit R = CH3, C2H5) werden nach bekannten Vorschriften aus CH2Cl2, Lithiumbutanid und HgCl2 bzw. CH3HgCl oder C2H5HgCl synthetisiert. Die 1H- und 13C-NMR- sowie die IR- und Ramanspektren der flüssigen Alkyle RHgCHCl2 und des hochschmelzenden Hg(CHCl2)2 werden registriert und ausgewertet. Nach der Röntgenstrukturanalyse kristallisiert Hg(CHCl2)2 in der monoklinen Raumgruppe P21/c mit 4 azentrischen Molekülen in der Elementarzelle (R = 0,046).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 441 (1978), S. 175-180 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of Tetramethyl(dimethylthiophosphinato)stiborane (CH3)4SbOP (S) (CH3)2(CH3)4SbOP(S)(CH3)2 crystallizes in the triclinic space-group P1 with a = 7.125, b = 9.297, c = 18.861 Å, α = 77.44°, ß = 83.86°, γ = 79.91° and four formula units per cell. Stibonium is distorted trigonal-bipyramidal and phosphorous distorted tetrahedral surrounded. The mean values of bondlengths are: Sb—Ceq = 2.108, Sb—Cax = 2.147, Sb—O = 2.641, P—C = 1.819, P—O = 1.514, and P—S = 1.987 Å.
    Notes: (CH3)4SbOP(S)(CH3)2 kristallisiert in der triklinen Raumgruppe P1 mit a = 7,125, b = 9,297, c = 18,861 Å, α = 77,44°,ß = 83,86°, γ = 79,91° und vier Formeleinheiten in der Zelle. Antimon ist verzerrt trigonal-bipyramidal und Phospor verzerrt tetraedrisch umgeben. Die Mittelwerte der Bindungsabstände sind: Sb—Cäq = 2,108, Sb—Cåx = 2,147, Sb—O = 2,641, P—C = 1,819, P—O = 1,514 und P—S = 1,987 Å.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 435 (1977), S. 179-190 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetramethyl Arsonium and Stibonium Methylchlorometallates of Gallium and IndiumThe preparation of the metallates of the general composition [Me4MV] + [Me4-xMIIIClx] - (with MV = As, Sb; MIII = Ga, In and x = 0-4) is described. The i.r., Raman, and 1H n.m.r. spectra of these ionic compounds are discussed. The results of the X-ray analysis of the monochloro complexes are given.
    Notes: Die Darstellung von Metallaten der allgemeinen Zusammensetzung [Me4MV] + [Me4-xMIIIClx] - (mit MV = As, Sb; MIII = Ga, In und x = 0-4) wird beschrieben. Die IR- Raman- und 1H-NMR-Spektren dieser ionisch gebauten Verbindungen werden diskutiert. Für die Monochlorokomplexe sind außerdem die Daten der Röntgenstrukturanalysen angegeben.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 429 (1977), S. 99-104 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of Dimeric DimethylaminodimethylindiumDimeric dimethylamino-dimethylindium was prepared by splitting off methane from the adduct Me3In—NHMe2 and characterized by its vibrational spectra. The structure - determined by X-ray analysis - has shown to have the monoclinic space group P21/c with a = 7.601, b = 7.336, c = 14.927 Å and β = 119.9°. Patterson, Fourier and Difference synthesis were used for determing the structure, which was refined by least square analysis to an R value of 0.068.
    Notes: Dimeres Dimethylamino-dimethylindium wurde durch Methanabspaltung aus dem Addukt Me3In—Me2NH dargestellt und schwingungsspektroskopisch charakterisiert. Die Röntgenstrukturanalyse führte zu der monoklinen Raumgruppe P21/c mit a = 7,601, b = 7,336, c = 14,927 Å und β = 119,9°. Die Struktur wurde aus Patterson-, Fourier- und Differenz-Fourier-Synthesen abgeleitet und nach der Methode der kleinsten Fehlerquadrate bis zu einem R-Wert von 0,068 verfeinert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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