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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: Crystal Structure of Tetracäsium-μ-oxo-decachlordiosmate(IV), Cs4[Os2OCl10]The anhydrous binuclear complex Cs4[Os2OCl10] crystallizes with an orthorhombic unit cell, Pcab, a = 12.521, b = 13.994, c = 11.798 Å and Z = 4 formula units. The complex anion forms corner sharing octahedrons tetragonally deformed. The interatomic distances are Os — O = 1.778 Å and Os — Cl = 2.370 (4×) and 2.433 Å (1×) respectively. The Cs atoms are coordinated differently. The interatomic distances Cs — Cl range from 3.46 to 3.87 Å. The structure is discussed in connection with analogous complexes. Details of other polynuclear complexes of Os are added.
    Notes: Der wasserfreie Zweikernkomplex Cs4[Os2OCl10] kristallisiert orthorhombisch in Pcab mit a = 12,521 Å, b = 13,994 Å, c = 11,798 und Z = 4 Formeleinheiten. Die komplexen Anionen bilden gestreckte, eckenverknüpfte Oktaeder mit Sauerstoff als Brückenatom. Die Bindungsabstände betragen Os — O = l,778 Å und Os — Cl = 2,370 Å (4×) bzw. 2,433 Å (1×). Die Cs-Atonie sind unterschiedlich koordiniert. Die Abstände Cs — Cl liegen im Bereich von 3,46 bis 3,87 Å. Die Struktur wird im Zusammenhang mit analogen Komplexen diskutiert. Es werden Angaben zu weiteren Mehrkernkomplexen des Os gemacht.
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon Sulphur Compounds. XXXIII. Structure of Bis (triphenylsilyl)sulphideThe condensation of triphenylsilanethiol yielded bis(triphenylsilyl)sulphide (1). The compound is remarkable resistent to hydrolysis. 1 crystallizes monoclinically [P21/n (No. 14): a = 1707.8 pm; b = 1454.6 pm; c = 1225.0 pm; β = 97.27°; Z = 4; 4470 h k l; R = 0.053]. The molecule is bent with a bond angle Si—S—Si = 112.0°. The mean bond distances Si—S and Si—C are 215.2 pm and 187.4 pm, respectively. Some structural details are discussed.
    Notes: Bis(triphenylsilyl)sulfid (1) wurde durch Kondensation von Triphenylsilanthiol erhalten. Die Verbindung ist bemerkenswert stabil gegen Hydrolyse. 1 kristallisiert monoklin [P21/n (Nr. 14); a = 1707,8 pm; b = 1454,6 pm; c = 1225,0 pm; β = 97,27°; Z = 4; 4470 hkl; R = 0,053]. Das Molekül ist gewinkelt mit einem Bindungswinkel Si—S—Si = 112,0°. Die Abstände Si—S bzw. Si—C betragen im Mittel 215,2 pm bzw. 187,4 pm. Die Einzelheiten der Struktur werden im Zusammenhang diskutiert.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydroxo Compounds. 12. Crystal Structure and Constitution of Sodium Trihydroxozincate Na[Zn(OH)3] 1The crystal structure of the very sensitive sodium trihydroxozincate Na[Zn(OH)3] 1 has been determined at 190 K. Contrary to the observations of trigonal planar [Zn(OH)3]- anions at 298 K, the structure of 1 at lower temperatures is characterized by 1-dimensional chains ∞1[Zn(OH)2(OH)2/2]- with the much more plausible (distorted) tetrahedral coordination of the Zn atoms (P42bc—C4v 6; Nr. 106; a = 1083.9 pm; c = 530.8 pm; Z = 8; Zn—O = 194.3-200.5 pm). The H positions were determined unambigeously from the X-ray data in complete agreement with calculations of potential profiles. There are pronounced hydrogen bond distances present. The Na atoms are coordinated by (5+1) oxygen atoms (Na—O = 234.8-248.8 pm and 282.7 pm). The noncentric coordination of the atoms as well as the strong anisotropic and anharmonic temperature tensors indicate a second order phase transition between 190 K and 298 K.
    Notes: Die Kristallstruktur des gegen Hydrolyse sehr empfindlichen Natriumtrihydroxozinkats Na[Zn(OH)3] 1 wurde bei 190 K bestimmt. Während bei 298 K trigonal-planare [Zn(OH)3]--Anionen beobachtet wurden, ist die Struktur von 1 bei tieferen Temperaturen durch 1-dimensionale Ketten ∞1[Zn(OH)2(OH)2/2]- mit der wesentlich plausibleren (verzerrten) Tetraederkoordination der Zn-Atome charakterisiert (P42bc—C4v 6; Nr. 106; a = 1083,9 pm; c = 530,8 pm; Z = 8; Zn—O = 194,3-200,5 pm). Die H-Positionen wurden in Übereinstimmung mit Berechnungen der Potentialprofile aus den Beugungsdaten bestimmt. Es treten ausgeprägte H-Brückenbindungen auf. Die Na-Atome sind von (5+1) O-Atomen koordiniert (Na—O = 234,8-248,8 pm, sowie 282,7 pm). Die azentrische Koordination aller Atome, sowie die anisotropen bzw. anharmonischen Tensoren lassen vermuten, daß zwischen 190 K und 298 K ein Phasenübergang 2. Ordnung stattfindet.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of TetraphenyldisiloxaneTetraphenyldisiloxane 1 crystallizes at 298 K monoclinically (P21/n; a = 1407.6; b = 610.7; c = 1262.7 pm; β = 95.87° Z = 2) and undergoes a second order phase transition at 200 K, in an almost unchanged structure of triclinic symmetry. At 298 K the molecules are already bent (Si—O—Si = 160°) with static or dynamical disorder of the bridging atom. Both Si—O distances are different (156 or 169 pm), because the shift of the bridging O atom is not perpendicular to the Si—to—Si vector. The reason for this remarkable behavior is not yet clear. According to the vibrational spectra, the Si—O—Si bridge is bent in the crystal but, in CCl4 solution a dynamical oscillation through the linear configuration may occur.
    Notes: Tetraphenyldisiloxan 1 kristallisiert bei 298 K monoklin (P21/n; a = 1407,6 pm; b = 610,7 pm; c = 1262,7 pm; β = 95,87° Z = 2) und durchläuft bei 200 K einen Phasenübergang 2. Ordnung in eine kaum veränderte Struktur trikliner Symmetrie. Bereits bei 298 K liegen in der Struktur gewinkelte Moleküle (Si—O—Si = 160°) mit statischer oder dynamischer Fehlordnung des Brückenatoms vor. Die beiden Abstände Si—O sind verschieden (156 bzw. 169 pm), weil die Auslenkung des Brückenatoms aus der zentralen Lage nicht senkrecht zum Vektor Si—Si erfolgt. Der Grund für dieses merkwürdige Verhalten ist unklar. Die Schwingungsspektren beweisen für den kristallinen Zustand ebenfalls die gewinkelte Struktur, während in CCl4-Lösungen ein dynamisches Durchschwingen durch die gestreckte Konfiguration wahrscheinlich ist.
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  • 5
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulphur Compounds. 53. Structure of 1,3-Dimethyl-1,1,3,3-tetraphenyldisilthiane1,3-Dimethyl-1,1,3,3-tetraphenyldisilthiane was obtained by an insertion reaction of sulphur with Ph2 MeSiH. The compound crystallizes triclinically (P1; a = 1166.7; b = 1231.1; c = 988.6 pm; α = 113.23; β = 90.34; γ = 112.43°; Z = 2). The X-ray structure analysis shows a bent configuration of the molecule with Si—S—Si = 108.7°. The results are discussed together with the structures of hexaphenyldisilthiane and dimethyltetraphenyldisiloxane.
    Notes: 1,3-Dimethyl-1,1,3,3-tetraphenyldisilthian entsteht aus Schwefel und Ph2MeSiH in einer Einschub-Reaktion. Die Verbindung kristallisiert triklin (P1; a = 1166,7; b = 1231,1; c = 988,6 pm; α = 113,23; β = 90,34; γ = 112,43°; Z = 2). Die Kristallstruktur-analyse ergab eine gewinkelte Konfiguration des Moleküls mit Si—S—Si = 180,7°. Die Ergebnisse werden im Zusammenhang mit der Struktur des Hexaphenyldisilthians und Dimethyltetraphenyl disiloxans diskutiert.
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  • 6
    ISSN: 0044-2313
    Keywords: Tetrahetero-tetrahedrane anions ; G44-, Sn44; ; infrared, Raman spectra; ; internal vibrations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Internal Vibration of the Tetrahetero-Tetrahedrane Anions Ge44-, Sn44-, and Pb44The Frequencies of the internal vibrations ν1 (A1), ν2(E), ν3(T2) of the tetrahetero-tetrahedrane an ions Ge44- and Sn44- are determined from the infrared and Raman spectra of K7LiGe8 and KSn, respectively. A comparison of the characteristic vibration of tetrahedrane anions X44- (X = Si, Ge, Sn)and the isoelectronic neutral tetrahedranes Y4 of the neighbouring elements (Y = P, As, Sb) shows a rather constant ratio of the corresponding frequencies k = v˜(X44-) = 0,77. This allows for an estimate of v˜(Pb44-) from the known Bi4data. In the inflated spectrum of KPb bands are observed in the predicted frequency range.
    Notes: Aus den Infrarot-und Raman-Spektren von K7LiGe8 und KSn werden die Frequenzen der inneren Schwingungen ν1(A1), ν2(E) und ν3(T3) der Tetrahetero-Tetrahedran -Anionen Ge44- und Sn44- bestimmt. Der Vergleich der charakteristischen Schwingungen von Tetrahedran-Anionen X44-(X = Si, Ge, Sn) und isoelektronischen neutralen Tetrahedranen Y4 der Nachbarelemente (Y = P,As, Sb)ergibt ein nahezu konstantes Verhältnis für die einander entsprechenden Frequenzen k = v˜(X44-)/v˜(Y4) = 0,77. Damit werden aus den Frequenzen v˜(Bi4) Werte für v˜(Pb44-) abgeschätzt, welche mit Banden im Infrarot-Spektrum von KPb übereinstimmen.
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  • 7
    ISSN: 0044-2313
    Keywords: K2Fe[P2S6] ; Hexathiodiphosphate(IV) ; Hexathiohypodiphosphate ; Crystal Structure ; Magnetism ; Vibrational Spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur, Magnetismus und Schwingungsspektrum von Dikaliumeisen(II)hexathiodiphosphat(IV), K2Fe[P2S6]K2Fe[P2S6] wurde aus den Elementen bei 1173 K in evakuierten, abgeschmolzenen Quarzampullen dargestellt. Die Verbindung bildet transparente, orangefarbene, luft- und feuchtigkeitsbeständige Kristalle. K2Fe[P2S6] kristallisiert monoklin, Raumgruppe P21/n (Nr. 14), mit den Gitterkonstanten (T = 298,5 K): a = 6,0622(4), b = 12,172(1) und c = 7,3787(8) Å, β = 101,113(7)°, Z = 2. Der neuartige Strukturtyp (mP22) wird durch Säulen von alternierend flächenverknüpften S6-Oktaedern und trigonalen Antiprismen (beide verzerrt) charakterisiert, die parallel zur a-Achse verlaufen und durch K+-Kationen (KZ 10; {2,6,2}-Polyeder; d(K—S) = 3,231 - 3,845 Å) miteinander verbunden sind. Die S6-Polyeder der Säulen werden alternierend durch Fe (d̄(Fe—S) = 2,577 Å) bzw. P2-Paare zentriert, die zur a-Achse um 73,4° geneigt sind. Die Bindungslängen in den Hexathiodiphosphat(IV)-Anionen [P2S6]4- mit angenäherter 32/m - D3d-Symmetrie betragen d(P—P) = 2,20 und d̄(P—S) = 2,02 Å. Die Titelverbindung ist oberhalb TN = 28 K paramagnetisch mit μ = 4,69 B.M. und ordnet unterhalb TN antiferromagnetisch. Die beobachteten inneren Moden der Raman- und Infrarotspektren von K2Fe[P2S6] stehen im Einklang mit der Faktorgruppenanalyse. Die Schwingungsbanden werden auf der Basis von [P2S6]4--Einheiten unter Berücksichtigung der Abweichungen von der D3d-Symmetrie zugeordnet.
    Notes: K2Fe[P2S6] was synthesized from the elements at 1173 K in sealed quartz tubes. The compound forms transparent orange crystals, stable against air and moisture. K2Fe[P2S6] crystallizes in the monoclinic system, space group P21/n (No. 14), with cell dimensions (T = 298.5 K) a = 6.0622(4), b = 12.172(1) and c = 7.3787(8) Å, β = 101.113(7)°, Z = 2. The novel structure type (mP22) is characterized by columns of alternating face-sharing S6 octahedra and trigonal antiprisms (both distorted) parallel to the a axis, which are interconnected by inserted K+ (CN 10; {2,6,2}-polyhedra; d(K—S) = 3.231 - 3.845 Å). The S6 polyhedra of the columns are centered alternately by Fe (d̄(Fe—S) = 2.577 Å) and P2 pairs which are inclined to the a axis by 73.4°. The bond lengths in the hexathiodiphosphate(IV) anions, [P2S6]4-, with approximate 3 2/m - D3d symmetry, are d̄(P—P) = 2.20 and d̄(P—S) = 2.02 Å. The compound is paramagnetic above TN = 28 K with μ = 4.69 B.M. and orders antiferromagnetically below TN. The internal modes of the observed Raman and FIR spectra of K2Fe[P2S6] are in accord with the factor group analysis, and the spectra are assigned on the basis of [P2S6]4- units, taking into account the deviation from D3d symmetry.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1035-1037 
    ISSN: 0044-2313
    Keywords: Titanium diboride ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: H—TiO or TiB2? - A CorrectionReinvestigations of “H—TiO” single crystals and the comparison with measurements of TiB2 crystals have shown that “H—TiO” in fact is titanium diboride.
    Notes: Eine erneute Untersuchung der Einkristalle von „H—TiO“ und der Vergleich mit Messungen an TiB2-Kristallen hat gezeigt, daß es sich bei „H—TiO“ um Titandiborid handelte.
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  • 9
    ISSN: 0044-2313
    Keywords: Li(THF)2[η2-(tBu2P)2P] ; Li(TMEDA)[η2-(tBu2P)2P] ; Li(THF)2[η2-(iPr2P)2P] ; Li(THF)2[η2-(Et2N)2P—P—PtBu2] ; Li(THF)2[η2-(tBu2P—P—PiPr2)] ; (tBu2P)2P—SiMe3 ; crystal structures ; 1H, 31P, 7Li-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation and Structure of Li(THF)2[η2-(tBu2P)2P], Li(TMEDA)[η2-(tBu2P)2P], Li(THF)2[η2-(iPr2P)2P], Li(THF)2[η2-(Et2N)2P—P—PtBu2], Li(THF)2[η2-(tBu2P—P—PiPr2] and (tBu2P)2P—SiMe3The formation and crystal structures of the compounds (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA)[η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 and Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 are reported. Compounds 3-6 are formed by reacting the corresponding silylated triphosphanes with nBuLi: 2 and 3 result from (tBu2P)2P—SiMe3 1, 4 from (iPrP)2P—SiMe3, 5 from (Et2N)2P—P(SiMe3)—PtBu2 and 6 from tBu2P—P(SiMe3)—PiPr2. 1 crystallizes in the orthorhombic space group P212121 (no. 19) with a = 910.87(7) pm, b = 1132.5(1) pm, c = 2373.5(2) pm (determined at 90 K). The structure determination of 2 was performed at 293 K and 200 K, respectively. 2 crystallizes in the monoclinic space group P21/n (no. 14) with a = 1069.7(3) pm, b = 1802.5(3) pm, c = 1604.0(7) pm, β = 98.11(2)° (200 K); 3 also in P21/n (no. 14) with a = 904.3(2) pm, b = 1936.4(5) pm, c = 1653.2(3) pm, β = 94.52(1)° (200 K). 4 crystallizes monoclinically in C2/c (no. 15) with a = 1650.0(5) pm, b = 945.6(3) pm, c = 1779.8(5) pm, β = 108.81(2)° (200 K); 5 in P21/n (no. 14) with a = 939.4(5) pm, b = 1736.8(6) pm, c = 1943.3(7) pm, β = 98.17(4)° (200 K). All compounds contain Z = 4 molecules in the unit cell.The 1H, 31P and 7Li NMR spectra of 2-6 are discussed.
    Notes: Es wird über die Verbindungen (tBu2P)2P—SiMe3 1, Li(THF)2[η2-(tBu2P)2P] 2, Li(TMEDA) · [η2-(tBu2P)2P] 3, Li(THF)2[η2-(iPr2P)2P] 4, Li(THF)2[η2-(Et2N)2P—P—PtBu2] 5 und Li(THF)2[η2-(tBu2P—P—PiPr2)] 6 berichtet. Letztere bilden sich durch Umsetzung der entsprechenden silylierten Triphosphane mit nBuLi: 2 und 3 aus (tBu2P)2P—SiMe3 1, 4 aus (iPr2P)2P—SiMe3, 5 aus (Et2N)2—P · (SiMe3)—PtBu2, 6 aus tBu2P—P(SiMe3)—PiPr2.1 kristallisiert orthorhombisch in P212121 (Nr. 19) mit a = 910,87(7) pm, b = 1132,5(1) pm, c = 2373,5(2) pm (bei 90 K bestimmt). Die Strukturbestimmung von 2 erfolgte bei 293 K und 200 K. 2 kristallisiert monoklin in P21/n (Nr. 14) mit a = 1069,7(3) pm, b = 1802,5(3) pm, c = 1604,0(7) pm, β = 98,11(2)° (200 K), 3 ebenfalls in P21/n (Nr. 14) mit a = 904,3(2) pm, b = 1936,4(5) pm, c = 1653,2(3) pm, β = 94,52(1)° (200 K). 4 kristallisiert monoklin in C2/c (Nr. 15) mit a = 1650,0(5) pm, b = 945,6(3) pm, c = 1779,8(5) pm, β = 108,81(2)° (200K), 5 in P21/n (Nr. 14) mit a = 939,4(5) pm, b = 1736,8(6) pm, c = 1943,3(7) pm, β = 98,17(4)° (200 K). Alle fünf Verbindungen enthalten jeweils vier Formeleinheiten in der Elementarzelle.Es wird über die Untersuchung der 1H-, 31P- und 7Li-NMR-Spektren der Verbindungen 2-6 berichtet.
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  • 10
    ISSN: 0044-2313
    Keywords: Alkali metal germanides and stannides ; Zintl cluster anions ; Vibrational spectra ; Thermal decomposition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The binary germanides M12Ge17 and M4Ge9 (M = Na, K, Rb, Cs) and the stannides M12Sn17 and M4Sn9 (M = K, Rb, Cs) were identified by a combination of direct synthesis, thermogravimetric analysis, vibrational spectroscopy, X-ray powder data and single crystal structure analysis. The M12E17 phases contain the cluster anions [E9]4- and [E4]4- in the ratio 1:2, forming a hierarchical structure with the cluster anions at the atomic positions of the hexagonal Laves phase MgZn2. Like the M4E4 phases, the M4Ge9 compounds are hierarchical derivatives of the cubic Cr3Si structure but with [Ge9]4- anions. The thermogravimetric analyses give strong evidence for the existence of at least one more phase with [E9]4- and [E4]4- clusters and of the clathrate phases M6E136 in addition to the well-known M8E44□2 chlathrates.
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