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  • 1
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    American Association for the Advancement of Science (AAAS)
    In: Science
    Publication Date: 2017-02-10
    Description: Author: Jake Yeston
    Keywords: Inorganic Chemistry
    Print ISSN: 0036-8075
    Electronic ISSN: 1095-9203
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Computer Science , Medicine , Natural Sciences in General , Physics
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  • 2
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    American Association for the Advancement of Science (AAAS)
    In: Science
    Publication Date: 2017-01-27
    Description: Author: Jake Yeston
    Keywords: Inorganic Chemistry
    Print ISSN: 0036-8075
    Electronic ISSN: 1095-9203
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Computer Science , Medicine , Natural Sciences in General , Physics
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  • 3
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    American Association for the Advancement of Science (AAAS)
    In: Science
    Publication Date: 2017-01-27
    Description: Polynitrogens have the potential for ultrahigh-performing explosives or propellants because singly or doubly bonded polynitrogens can decompose to triply bonded dinitrogen (N2) with an extraordinarily large energy release. The large energy content and relatively low activation energy toward decomposition makes the synthesis of a stable polynitrogen allotrope an extraordinary challenge. Many elements exist in different forms (allotropes)—for example, carbon can exist as graphite, diamond, buckyballs, or graphene. However, no stable neutral allotropes are known for nitrogen, and only two stable homonuclear polynitrogen ions had been isolated until now—namely, the N3− anion (1) and the N5+ cation (2). On page 374 of this issue, Zhang et al. (3) report the synthesis and characterization of the first stable salt of the cyclo-N5− anion, only the third stable homonuclear polynitrogen ion ever isolated. Author: Karl O. Christe
    Keywords: Inorganic Chemistry
    Print ISSN: 0036-8075
    Electronic ISSN: 1095-9203
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Computer Science , Medicine , Natural Sciences in General , Physics
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  • 4
    Keywords: Life sciences ; Chemistry, Inorganic ; Bioorganic chemistry ; Emerging infectious diseases ; RNA-ligand interactions ; Microbiology ; Life sciences ; Microbiology ; Protein-Ligand Interactions ; Inorganic Chemistry ; Bioorganic chemistry ; Infectious Diseases ; Springer eBooks
    Description / Table of Contents: A History of Iron Metabolism in the Mycobacteria -- Mycobacterial Iron Uptake Mechanisms -- Siderocalin Combats Mycobacterial Infections -- Design of Anti-TB Drugs Using the Iron Uptake Platform
    Abstract: Iron Acquisition by the Genus Mycobacterium summarizes the early evidence for the necessity of iron in mycobacteria and the discovery of the mycobacterial siderophores mycobactin, carboxymycobactin, and exochelin. The structural characterization of the mycobacterial siderophores is described. ℗ The genes so far identified as essential for iron acquisition and maintenance of an infection by pathogenic mycobacteria are discussed.℗ The potential role of siderocalin in iron gathering by M. tuberculosis is featured. Because new drugs for M. tuberculosis are needed, this brief also emphasizes the design of antibiotics that interfere with siderophore biosynthesis and the use of siderophore analogs and/or conjugates
    Pages: : digital.
    ISBN: 9783319003030
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  • 5
    Dordrecht : Springer Science+Business Media B.V.
    Keywords: Medicine ; Chemistry, Inorganic ; Cytology ; Environmental toxicology ; Biomedicine ; Biomedicine general ; Cell Biology ; Oxidative Stress ; Apoptosis ; Ecotoxicology ; Inorganic Chemistry ; Springer eBooks
    Pages: : digital
    ISBN: 9789400704282
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  • 6
    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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  • 7
    ISSN: 0044-2313
    Keywords: 2,2′,3,3′,4,4′-hexatertiarybutyl-1,1′-bicyclotetraarsane ; arsenic polycycles ; structural isomers ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: tBu6As8 - a Compound of Known Composition and New StructureThe compound 2,2′,3,3′,4,4′-hexatertiarybutyl-1,1′-bicyclotetraarsane (1) can be obtained in good yields through the reaction of (tBuAs)4 with [Co2(CO)8]. 1 is the structural isomer of 2,3,4,6,7,8-hexatertiarybutylbicyclo-[3.3.0]octaarsane (2) described in 1981 by Baudler et al. [3]. 1 was characterized by 1H-NMR spectroscopy, mass spectroscopy and crystal structure analysis. Isomerisation into 2 can be observed, by tempering a solution of 1 in toluene for ten hours at 90°C.
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  • 8
    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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  • 9
    Electronic Resource
    Weinheim : Wiley-Blackwell
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 10
    ISSN: 0044-2313
    Keywords: Iodyldisulfate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Crystal Structure Analysis of an Iodyl CompoundSingle crystals of (IO2)2S2O7 were obtained for the first time by reacting iodic acid and oleum at 195°C. According to the results of a X-ray structure determination (monoclinic, P21/a, a = 885.0(2), b = 1037.3(2), c = 915.8(2) pm, β = 94.75(2)°, Z = 4, 1466 diffractometer data, R1 = 0.033, wR2 = 0.063), (IO2)2S2O7 contains dimeric iodyl cations (IO2)22+, which are connected by disulfate groups thus forming polymeric strands. Strikingly, the I—O-distances range almost continously from 174 pm (strong intramolecular bonds) to — 300 pm (van der Waals contacts).
    Notes: Durch Umsetzung von Iodsäure in Oleum bei 195°C wurden erstmals Einkristalle von Iodyldisulfat erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/a, a = 885,0(2), b = 1037,3(2), c = 915,8(2) pm, β = 94,75(2)°, Z = 4, 1466 unabhängige Reflexe, R1 = 0,033, wR2 = 0,063) liegen dimere Iodylkationen (IO2)22+ vor, die über Disulfatgruppen zu polymeren Strängen verknüpft sind. Auffällig ist eine nahezu gleichmäßige Verteilung der I—O-Abstände über den gesamten Bereich von starken intramolekularen Bindungen (174 pm) bis zu intermolekularen Kontakten vom van der Waals Typ (> 300 pm).
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  • 11
    ISSN: 0044-2313
    Keywords: 31P NMR ; triphospha arsena trichalcogena diiodide ; triphospha arsena trithia diiodomethyl iodide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Derivatives of Arsenic Substituted Phosphorus Chalcogenidesα-AsP3S3I2, α-AsP3Se3I2, and three isomers of β-AsP3S3I2 were observed besides several phosphorus sulfides by 31P NMR spectroscopy after the reaction of AsnP4-nE3 (E = S; Se; n = 0-4) with I2 in the melt or with I2, PI3, and N-iodosuccinimid in CS2 solutions. The reaction of AsnP4-nS3 with CHI3 in CS2 solution yielded two isomers of β-AsP3S3(CHI2)I.
    Notes: Nach der Reaktion von AsnP4-nE3 (E = S; Se; n = 0-4) Gemischen mit I2 in der Schmelze oder mit I2, PI3 oder N-Iodsuccinimid in CS2-Lösungen konnten durch 31P-NMR-Spektroskopie Abbauprodukte wie Phosphorsulfide, aber auch Derivate des Edukts, nämlich α-AsP3S3I2, α-AsP3Se3I2 und β-AsP3S3I2, letzteres mit drei Isomeren, identifiziert werden. Bei der Reaktion von CHI3 mit AsnP4-nS3 entstanden zwei Isomere von β-AsP3S3(CHI2)I.
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  • 12
    ISSN: 0044-2313
    Keywords: Lithium ; Rare Earth Halides ; Crystal Structures ; Ionic Motion ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Halides of the A3MX6 Type. VI. Ternary Chlorides of the Rare-Earth Elements with Lithium, Li3MCl6 (M = Tb—Lu, Y, Sc): Synthesis, Crystal Structures, and Ionic MotionSingle crystal X-ray studies on the ternary chlorides Li3ErCl6, Li3YbCl6 and Li3ScCl6 show that they crystallize in three different structure types. Li3ErCl6 (trigonal, P3ml, Z = 3, a = 1117.7(2); c = 603.6(2) pm; the chlorides with M = Tb—Tm, Y are isotypic) and Li3YbCl6 (orthorhombic, Pnma, Z = 4, a = 1286.6(1); b = 1113.2(1); c = 602.95(8) pm; Li3LuCl6 is isotypic) have very similar structures that may be derived from hexagonal closest packings of chloride ions with the cations occupying octahedral holes in part statistically. Li3ScCl6 (monoclinic, C2/m, Z = 2, a = 639.8(1); b = 1104.0(2); c = 639,1(1) pm; β = 109.89(1)°) crystallizes isotypic with Na3GdI6 and Li3ErBr6, structures that may be derived from a cubic closes packings of anions. The ionic movement in Li3YCl6 and Li3YbCl6 has been investigated by impedance and 7Li-NMR spectroscopy.
    Notes: Die ternären Chloride Li3ErCl6, Li3YbCl6 und Li3ScCl6 kristallisieren nach röntgenographischen Untersuchungen an Einkristallen in drei verschiedenen Strukturtypen. Li3ErCl6 (trigonal, P3ml, Z = 3, a = 1117,7(2); c = 603,6(2) pm; isotyp mit M = Tb—Tm, Y) und Li3YbCl6 (orthorhombisch, Pnma, Z = 4, a = 1286,6(1); b = 1113,2(1); c = 602,95(8) pm; Li3LuCl6 ist isotyp) haben sehr ähnliche Strukturen, die sich als hexagonal-dichteste Kugelpackungen von Chlorid-Ionen mit zum Teil statistischer Auffüllung der Oktaederlücken mit Kationen beschreiben lassen. Li3ScCl6 (monoklin, C2/m, Z = 2, a = 639,8(1); b = 1104,0(2); c = 639,1(1) pm; β = 109,89(1)°) kristallisiert isotyp mit Na3GdI6 und Li3ErBr6; die Anionen bilden hier eine kubisch-dichteste Kugelpackung. Die Ionenbewegung in Li3YCl6 und Li3YbCl6 wurde mittels Impedanzspektroskopie und 7Li-NMR-Spektroskopie untersucht.
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  • 13
    ISSN: 0044-2313
    Keywords: Titanium compound ; Phosphorane iminato derivatives ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrakis(triphenylphosphoraneiminato)titanium, [Ti(NPPh3)4]The title compound has been prepared by the reaction of [TiCl2(NPPh3)2] with methyllithium and cyclopentadienyllithium, respectively, in hexane solution. [Ti(NPPh3)4] · 3 C7H8 crystallizes from toluene solution to form colourless, only slightly moisture sensitive crystals which were characterized by a crystal structure determination. Space group I41/a, Z = 8, lattice dimensions at -80°C: a = b = 2160.7(2), c = 3334.2(3) pm, merohedral (110) twin, R = 0.077. The compound forms monomeric molecules with tetrahedrally coordinate titanium atoms and bonding parameters of TiN = 187.3 pm, PN = 155.1 pm, TiNP 150.4° in average.
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  • 14
    ISSN: 0044-2313
    Keywords: Magnesium Compounds ; Phosphoraneiminato Complexes ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphaneimine and Phosphoraneiminato Complexes of Magnesium. The Crystal Structures of [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2], [Mg2I2(Me3SiNPMe2CH2)(Me3SiNPMe2CH2CH(Me)O)(OEt2)], and [MgBr(NPMe3)]4 · C7H8By reactions of the silylated phosphaneimine Me3SiNPMe3 with the Grignard reagents EtMgBr and MeMgI, respectively, the carbanionic phosphoraneiminato derivatives [XMg(CH2PMe2NSiMe3)]n (X = Br, I) can be isolated as main products. The by-products of these reactions, [MgBr1.25I0.75(Me3SiNPMe3)(OEt2)], [MgI2(Me3SiNPMe3)2] and [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3)(OEt2)] were identified by crystal structure determinations. The phosphoraneiminato complex [MgBr(NPMe3)]4 · C7H8 with hetero cubane structure is formed by a metathesis reaction of [ZnBr(NPMe3)]4 with RMgBr (R = Ph. Mes).
    Notes: Als Hauptprodukte der Umsetzungen des silylierten Phosphanimins Me3SiNPMe3 mit den Grignard-Reagentien EtMgBr und MeMgl wurden die carbanionischen Phosphaniminato-Derivate [XMg(CH2Pme2NSiMe3)]n (X = Br, I) isoliert. Als Nebenprodukte wurden [MgBr1,25I0,75(Me3SiNPMe3)(OEt2)], [Mgl2(Me3SiNPMe3)2] und [Mg2I2(CH2PMe2NSiMe3)(O(Me)CHCH2PMe2NSiMe3(OEt2)] durch röntgenographische Strukturanalysen identifiziert. Den Phosphaniminato-Komplex [MgBr(NPMe3)]4 · C7H8 mit Heterocuban-Struktur erhielten wir durch Metathese-Reaktion aus [ZnBr(NPMe3)]4 und RMgBr (R = Ph, Mes).
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  • 15
    ISSN: 0044-2313
    Keywords: [η2-{tBu2P—P=PtBu2} PtBr(PPh3)] ; crystal structure ; 1H-, 13C-, 31P-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Coordination Chemistry of P-rich Phosphanes and Silylphosphanes. XIII [1]. [η2-{tBu2P—P=PtBu2} PtBr(PPh3)][η2-{tBu2P—P=PtBu2} PtBr(PPh3)] 1 is the first transition metal complex compound resulting from a phosphino-phosphinidene-phosphorane. The yellow crystals of 1 (fp. 201-203°C, decomp.) were obtained by reacting tBu2P—P=P(Br)tBu2 with either (Ph3P)2Pt · C2H4, or with Pt(PPh3)4, resp. Compound 1 crystallizes triclinic in the space group P1 (no. 2) with a = 1076.80(8) pm, b = 1344.61(8) pm, c = 1381.16(9) pm, α = 81.773(6)°, β; = 85,110(8), γ = 88,776(7).
    Notes: [η2-{tBu2P—P=PtBu2} PtBr(PPh3)] 1 ist die erste Komplexverbindung aus einem Phosphino-phosphiniden-phosphoran. Die gelben Kristalle von 1, Smp. 201-203°C (unter Zersetzung) bilden sich bei der Umsetzung von tBu2P—P=P(Br)tBu2 mit (Ph3P)2Pt · C2H4 oder Pt(PPh3)4. 1 kristallisiert triklin in P1 (Nr. 2) mit a = 1076,80(8) pm, b = 1344,61(8) pm, c = 1381,16(9) pm, α = 81,773(6)°, β; = 85,110(8)°, γ = 88,776(7).
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  • 16
    ISSN: 0044-2313
    Keywords: (Borylorganyl)phosphanes ; (Borylorganyl)phosphoniumsalt ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese und Reaktionen von {o-{[Bis(dimethylamino)boryl]methyl}phenyl}diphenyl-phosphanDas neue α,ω-[Boryl(organyl)]phosphan o-Ph2PC6H4CH2 (NMe2)2 (10) wurde synthetisiert und spektroskopisch charakterisiert. Die Reaktivität dieser Verbindung, vor allem gegenüber Substitutionsreaktionen am Boratom war der Gegenstand unserer Untersuchungen. Verbindung 10 reagiert mit MeOH, BCl3 bzw. HCl zu den Verbindungen o-Ph2PC6H4CH2B(OMe)2 (10 a), o-Ph2PC6H4CH2BCl2 (10 c), o-Ph2PC6H4CH2BCl2 (HNMe2) (10 d) und o-Ph2P(HCl)C6H4CH2 BCl2(HNMe2) (10 e). Die Umsetzung von 10 a mit LiAlH4 führt zu o-Ph2PC6H4CH2BH2 (10 b). Verbindung 10 e wurde zusätzlich durch eine Röntgenstrukturanalyse charakterisiert.
    Notes: The new α,ω-[boryl(organyl)]phosphane o-Ph2PC6H4CH2B (NMe2)2 (10) was obtained in good yields from the reaction of CIB(NMe2)2 with o-Ph2PC6H4CH2Li(tmeda). Five derivatives of 10 were obtained by substituting the boron-bound amino groups by reactions with MeOH, BCl3, HCl, and LiAlH4, respectively, in particular, o-Ph2(HCl)PC6H4CH2BCl2 (HNMe2) (10 e) which shows a unique P—H—Cl—H—N unit. Compound 10 and its derivatives were characterized by multinuclear NMR methods, mass spectra, and elemental analyses. In addition, the structure of 10 e · 1.5 C6H6 was determined by single crystal X-ray diffraction.
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  • 17
    ISSN: 0044-2313
    Keywords: Methylboratabenzene indium ; conformational variability ; automerization ; crystal packing effects ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Borabenzene Derivatives. 25 [1]. Methylbis(1-methylboratabenzene)indium: Synthesis and Structure. An Example for the Variability of Soft Structural Parameters in the Crystalline EnvironmentThe new boratabenzene derivative InMe(C5H5BMe)2 has been synthesized from 2-(Me3Sn)C5H5BMe and InMe3. The compound proves fluxional on the nmr time scale with average C2v symmetry in solution. An x-ray structure determination shows the existence of four molecules in the asymmetric unit differing mainly in the bonding geometry of the metal atoms with respect to the eight symmetrically independent boratabenzene ligands. Thus the dynamical behaviour in solution is reflected in the solid state by the soft structural parameters of the indium-ring coordination, with their variability exceeding the standard deviations of the corresponding individual observations by an order of magnitude.
    Notes: Ausgehend von 2-(Me3Sn)C5H5BMe und InMe3 wurde der neue Boratabenzol-Komplex InMe(C5H5BMe)2 erhalten. Die Verbindung zeigt in Lösung auf der NMR-Zeitskala eine fluktuierende Struktur mit effektiver C2v-Symmetrie. Die Kristallstrukturanalyse zeigt, daß im Festkörper vier Moleküle in der asymmetrischen Einheit vorliegen, die sich vorwiegend in der Bindung des Metallatoms an die insgesamt acht symmetrieunabhängigen Boratabenzol-Liganden unterscheiden. Das in Lösung dynamische Verhalten findet im Kristall seine Entsprechung in weichen Strukturparametern bezüglich der Indium-Ring-ligand-Koordination, deren Variabilität die Standardabweichungen der Einzelbeobachtung um eine Größenordnung übersteigt.
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  • 18
    ISSN: 0044-2313
    Keywords: Potassium tetraamido zincate ; X-ray structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Positions of the Protons in Potassium Tetraamidozincate, K2Zn(NH2)4X-ray single crystal data for K2Zn(NH2)4 allowed the determination of the so far unknown positions of the protons: P1, Z = 2, a = 6.730(1) Å, b = 7.438(1) Å, c = 8.019(2) Å, α = 72.03(2)°, β = 84.45(2)°, γ = 63.82(1)°, Z(F0) with (F0)2 ≥ 3σ(F0)2 = 2166, Z(parameters) = 96, R/RW = 0.032/0.039.In the structure of K2Zn(NH2)2 the amide ions are nearly hexagonal close packed. One layer of octahedral holes parallel to (010) is fully occupied by potassium atoms and zinc is in an ordered way in a quarter of the tetrahedral holes of the next layer. The orientation of the protons of the amide ions is characteristic for this type of structure (filled up CdI2 type).
    Notes: Die bisher unbekannten Protonenlagen bei K2Zn(NH2)4 wurden röntgenographisch über Einkristalldaten bestimmt: P1, Z = 2, a = 6,730(1) Å, b = 7,438(1) Å, c = 8,019(2) Å, α = 72,03(2)°, β = 84,45(2)°, γ = 63,82(1)°, Z(F0) mit (F0)2 ≥ 3σ(F0)2 = 2166, Z(Parameter) = 96, R/RW = 0,032/0,039.Die Amidionen bilden das Motiv einer hexagonal dichtesten Kugelpackung. Darin sind in Ebenen parallel (010) abwechselnd alle Oktaederlücken durch Kalium oder geordnet 1/4 der Tetraederlücken durch Zink besetzt. Die Orientierung der Protonen an den Amidionen ist für diesen Strukturtyp (aufgefüllter CdI2-Typ) charakteristisch.
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  • 19
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1108-1112 
    ISSN: 0044-2313
    Keywords: Sodium tetra amido manganate(II) ; sodium manganese (II) amide ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na2Mn(NH2)4: A New Type of Layered StructureThe structure of Na2Mn(NH2)4 was solved by X-ray single crystal data including H-positions: P21/c, Z = 4, a = 6.331(1) Å, b = 14.542(3) Å, c = 7.212(1) Å, β = 116.29(1)°, Z(F20 ≥ 3σ = (F20)) = 1343, Z(parameters) = 96, R/RW = 0.023/0.029.The compound crystallizes in a new type of structure. Within layered blocks the amide ions are arranged with the motif of a hexagonal closest packing of spheres. Within these blocks alternating layers contain sodium in all octahedral sites and manganese in an ordered way in a quarter of tetrahedral sites.
    Notes: Die Struktur von Na2Mn(NH2)4 wurde röntgenograhisch über Einkristalldaten einschließlich der H-Lagen bestimmt: P21/c, Z = 4, a = 6,331(1) Å, b = 14,542(3) Å, c = 7,212(1) Å, β = 116,29(1)°, Z(F0) mit (F0)2 ≥ 3σ(F0)2 = 1343, Z(Parameter) = 96, R/RW = 0,023/0,029.Die Verbindung kristallisiert in einem neuen Strukturtyp. Die Amidionen bilden innerhalb von Schichtenpaketen das Motiv einer hexagonal dichtesten Kugelpackung. In ihr sind in einzelnen Ebenen abwechselnd entweder alle Oktaederlücken durch Natrium oder geordnet 1/4 der Tetraederlücken durch Mangan besetzt.
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  • 20
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Structures of the Phosphorus and Nitrogenbridged Transition Metal Complexes [Pd(NPhPPh2)(PPh3)]2, [Pd(NPhPPh2)2 · Li(thf)]2, [Pd(NPhPPh2)Cl · Li(thf)3]2, [M(NPhPPh2)(HNPhPPh2)]2 (M=Pd, Pt), [M{Ph2P(NPh)2}2] (M=Co, Ni), [Ni(PPh2){Ph2P(NPh)2}]2 and [Ni2(PPh2)(NPhPPh2)(HNPhPPh2)3].From the reaction of LiNPhPPh2 with Palladium-Nickel- and Cobaltcomplexes, depending on the reaction conditions, different monomeric and dimeric complexes can be isolated. In these compounds the (NPhPPh2)--group acts as both a bridging and as a terminal ligand. [Pd(NPhPPh2)(PPh3)]2 (1), [Pd(NPhPPh2)2 · Li(thf)]2 (2) and [Pd(NPhPPh2)Cl · Li(thf)3]2 (3) are formed from the reaction of [PdCl2(PPh3)2] or [PdCl2(COD)] with LiNPhPPh2. In contrast to this from the reaction of Pd(Ac)2 and HNPhPPh2 (in the presence of zinc-dust) or [PtCl2(py)2] and LiNPhPPh2.
    Notes: Bei der Reaktion von LiNPhPPh2 mit Komplexen des Palladium, Cobalt und Nickel können je nach den Reaktionsbedingungen unterschiedliche einkernige und zweikernige Komplexe isoliert werden, in denen die (NPhPPh2)--Gruppe als Brücke bzw. endständiger Ligand vorliegt. [Pd(NPhPPh2)(PPh3)]2 (1), [Pd(NPhPPh2)2 · Li(thf)]2 (2) und [Pd(NPhPPh2)Cl · Li(thf)3]2 (3) werden bei der Umsetzung von [PdCl2(PPh3)2] bzw. [PdCl2(COD)] mit LiNPhPPh2 gebildet. Dagegen erhält man aus Pd(Ac)2 und HNPhPPh2 (in Gegenwart von Zinkstaub) bzw. [PtCl2(py)2] und LiNPhPPh2 die zweikernigen Komplexe [M(NPhPPh2)(HNPhPPh2)]2 (M = Pd: 4; M = Pt: 5). Die Umsetzung von [MCl2(PR3)2] (M = Ni: R = Ph, iPr; M = Co: R = Ph) führt dagegen zur Bildung der einkernigen Verbindungen [M{Ph2P(NPh)2}2] (M = Ni: 6; M = Co: 7) und des zweikernigen Komplexes [Ni(PPh2){Ph2P(NPh)2}]2 (8). Wird [NiCl2(PPh3)2] mit HNPhPPh2 in Gegenwart von Zinkstaub zur Reaktion gebracht, entsteht [Ni2(PPh2)(NPhPPh2)(HNPhPPh2)3] (9). Die Strukturen von 1-9 konnten mit Hilfe der Röntgenstrukturanalyse aufgeklärt werden. 1-9 besitzen folgende Gitterkonstanten und Raumgruppen:(1: Raumgruppe P1 (Nr. 2), Z = 2, a = 1193,0(4) pm, b = 1325,5(5) pm, c = 1447,2(7) pm, α = 97,01(3)°, β = 112,69(3)°, γ = 115,75(3)°; 2: Raumgruppe P1 (Nr. 2), Z = 2, a = 1264,1(13) pm, b = 1281,7(12) pm, c = 1448,0(2) pm, α = 113,01(6)°, β = 92,99(8)°, γ = 117,28(8)°; 3: Raumgruppe P1 (Nr.2) Z = 2, a = 1094,3(8) pm, b = 1197,5(12) pm, c = 1313,7(17) pm, α = 110,22(6)°, β = 101,33(6)°, γ = 106,45(5)°; 4: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1490,1(4) pm, b = 1336,0(3) pm, c = 1746,9(6) pm, β = 97,52(3)°; 5: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1486,7(2) pm, b = 1332,0(10) pm, c = 1749,0(2), β = 97,65(10)°, 6: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1114,2(2) pm, b = 1722,7(3) pm, c = 2104,6(4) pm, β = 98,70(3); 7: Raumgruppe C2/c (Nr. 15), Z = 4, a = 1110,1(2) pm, b = 1714,3(3) pm, c = 2090,8(4) pm, β = 98,38(3)°; 8: Raumgruppe P1 (Nr. 2), Z = 2, a = 984,40(7) pm, b = 1189,7(8) pm, c = 1412,2(8) pm, γ = 101,49(5)°, β = 97,81(5), γ = 109,24(5); 9: Raumgruppe P1 (Nr. 2), Z = 2, a = 1402,1(9) pm, b = 1416,9(13) pm, c = 2230,0(2) pm, γ = 84,67(7)°, β = 84,98(6)°, γ = 65,72(6)°).
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  • 21
    ISSN: 0044-2313
    Keywords: Lithium ; imidazole derivatives ; peroxo complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Imidazole Derivatives. XXIV. [Li12O2Cl2(ImN)8(THF)4] · 8 THF: a Peroxo Lithium Fragment in a Novel Cage Structure1,3-dimethyl-2-iminoimidazoline (8, ImNH) reacts with methyl lithium to give [ImNLi]n (9). In tetrahydrofuran, crystals of C56H96Cl2Li12N24O6 · 8 C4H8O (10) are obtained. The structure of 10 consists of a Li12Cl2N8O2 core in which a peroxo unit is incorporated into a stack of ladder fragments. Over all, four tetrahydrofuran and eight imidazoline ligands are attached at the lithium and nitrogen atoms.
    Notes: 1,3-Dimethyl-2-iminoimidazolin (8, ImNH) reagiert mit Methyllithium in Diethylether zu [ImNLi]n (9). In Tetrahydrofuran werden Kristalle von [Li12O2Cl2(ImN)8(THF)4] · 8 THF (10) erhalten. In 10 liegt ein Li12Cl2N8O2-Käfig in Form gestapelter Leiterfragmente mit O22 als zentraler Einheit vor. Hieran sind über die Lithium- und Stickstoffatome insgesamt vier Tetrahydrofuran- und acht Imidazolin-Liganden koordiniert.
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  • 22
    ISSN: 0044-2313
    Keywords: Potassium dithiocarbiminate ; dithiolates ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of [ImNCS2K] (ImN = 1,3-Dimethylimidazoline-2-imino): a Novel Potassium DithiocarbiminateThe reaction of the 2-iminoimidazoline 4 with KMe gives the potassium imidate 7 from which the potassium 1,1-dithiolate 8 is obtained in almost quantitative yield. Crystals of C6H8N3S2K · 1/6 CH3CN (8 · 1/6 CH3CN) are triclinic, space group P1, Z = 6, a = 10.988(4), b = 13.597(8), c = 13.622(9) Å, α = 113.003, β = 105.53(3), γ = 105.62(3)°, V = 1636.90 Å3. The structure consists of a complicated 3-dimensional framework in which the K2 units bridged by the four sulfur atoms of two thiolate ligands are connected by nitrogen and sulfur bridges.
    Notes: Die Umsetzung des 2-Iminoimidazolins 4 mit KMe ergibt das Kaliumimidat 7, aus dem das Kalium-1,1-dithiolat 8 in fast quantitativer Ausbeute erhältlich ist. C6H8N3S2K · 1/6 CH3CN (8 · 1/6 CH3CN) kristallisiert triklin, Raumgruppe P1, Z = 6, a = 10.988(4), b = 13.597(8), c = 13.622(9) Å, α = 113.00(3), β = 105.53(3), γ = 105.62(3)°, V = 1636.90 Å3. Die komplexe Raumnetzstruktur besteht aus den durch die 4 Schwefelatome zweier Dithiolat-Liganden verbrückten K2-Einheiten, die ihrerseits über Stickstoff- und Schwefelatome verbunden sind.
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  • 23
    ISSN: 0044-2313
    Keywords: Bismuth ruthenium bromide ; bismuth ruthenium iodide ; subhalide ; crystal structure ; chemical bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi4RuBr2 and Bi4RuI2: Two Varieties of a Column Structure with Face-Sharing [RuBi8/2] Square AntiprismsReaction of the elements yields black, lustrous, air insensitive crystals of the subhalides Bi4RuI2 (tetragonal, I4/m, a = 1183.9(2) pm, c = 669.7(2) pm, V = 938.66 · 106 pm3) and Bi4RuBr2 (monoclinic, I112/m, a = 1211.9(2) pm, b = 1072.6(2) pm, c = 663.9(2) pm, γ = 91.63(1)°, V = 862.64 · 106 pm3). The structures of the homöotypic compounds contain ∞1[RuBi8/2] strands of face-sharing square antiprisms. Halogen atoms lie above the edges of alternate Bi4 squares. Thereby chemical bonding differs significantly within the two types of Bi4 squares. Though the Ru atoms on the central axis of the strand of antiprisms form pairs, extended Hückel calculations give no evidence of Ru—Ru bonds.
    Notes: Durch Umsetzung der Elemente werden schwarze, metallisch glänzende, luftstabile Kristalle der Subhalogenide Bi4RuI2 (tetragonal, I4/m, a = 1183,9(2) pm, c = 669,7(2) pm, V = 938,66 · 106 pm3) und Bi4RuBr2 (monoklin, I112/m,a = 1211,9(2) pm, b = 1072,6(2) pm, c = 663,9(2) pm, γ = 91,63(1)°, V = 862,64 · 106 pm3) erhalten. In den Strukturen der homöotypen Verbindungen liegen ∞1[RuBi8/2]-Stränge aus flächenverknüpften, quadratischen Antiprismen vor. Die Kanten jedes zweiten Bi4-Quadrates in einer Säule sind mit Halogenatomen überbrückt. Dadurch unterscheiden sich die Bindungsverhältnisse in den beiden Sorten von Bi4-Quadraten wesentlich. Die Ru-Atome auf der zentralen Achse des Antiprismenstranges bilden Paare, doch liegen nach Extended-Hückel-Rechnungen keine Ru—Ru-Bindungen vor.
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  • 24
    ISSN: 0044-2313
    Keywords: Bismuth ruthenium bromide ; subhalide ; cluster ; crystal structure ; pseudo-symmetry ; twinning ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi24Ru3Br20: A Pseudo-Tetragonal Structure with [RuBi6Br12] Clusters and [Ru2Bi17Br4] GroupsThe melting reaction of Ru with Bi and BiBr yields black, lustrous, air insensitive crystals of the subbromide Bi24Ru3Br20. The orthorhombic crystal structure (space group Pc21n, a = b = 1377.8(1) pm, c = 3222.3(4) pm, V = 6117.0 · 106 pm3) deceives pseudo-symmetry with respect to the tetragonal space group P4/ncc leading to multiply twinned crystals. The structure can formally be subdivided in [RuBi6Br12] clusters, [Ru2Bi17Br4] stacks, and [BiBr4] groups.
    Notes: Aus der Schmelzreaktion von Ru mit Bi und BiBr3 werden schwarze, metallisch glänzende und luftbeständige Kristalle des Subbromids Bi24Ru3Br20 erhalten. Die orthorhombische Kristallstruktur (Raumgruppe Pc21n, a = b = 1377,8(1) pm, c = 3222,3(4) pm, V = 6117,0 · 106 pm3) täuscht die Pseudosymmetrie der tetragonalen Raumgruppe P4/ncc vor, was zu mehrfach verzwillingten Kristallen führt. Die Struktur läßt sich formal in [RuBi6Br12]-Cluster, [Ru2Bi17Br4]-Stapel und [BiBr4]-Gruppen aufgliedern.
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  • 25
    ISSN: 0044-2313
    Keywords: Cyclophosphazenes ; [3]ferrocenophanes ; 1,1′-ferrocene-dichalcogenato compounds ; NMR spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Ferrocenol and 1,1′-Ferrocendiol with Cyclotriphosphazenes, P3N3F6 and P3N3Cl6The hexahalogeno-cyclotriphosphazenes, P3N3X6 (X = F (1 a), Cl (1 b)), react with ferrocenol (FcOH) in a molar ratio 1 : 1 to give the ferrocenoxy derivatives, FcO[P3N3X5] (X = F (3 a), Cl (3 b)); in an analogous manner the tetrameric ring P4N4Cl8 (2 b) is converted to FcO[P4N4Cl7] (4 b). Abkürzungen: Fc = Ferrocenyl, (C5H5)Fe(C5H4-); fc = 1,1′-ferrocendiyl, Fe(C5H4-)2; rc = 1,1′-ruthenocendiyl, Ru(C5H4-)2. Fluorphosphazene werden mit a, Chlorphosphazene mit b gekennzeichnet. With 1,1′-ferrocenediol, (fc(OH) 2), the cyclo triphosphazenes react in a molar ratio 1 : 1 to produce fcO 2[P 3 N 3 X 4] (X = F ( 5 a), Cl ( 5 b)). According to the x-ray structure analysis, the 1,1′-ferrocenediolato group in 5 a , b is bound to two different phosphorus atoms. On the contrary, the 1,1′-ferrocenedithiolato- and 1,1′-ferrocenediselenolato units in fcS 2[P 3 N 3 X 5] (X = F ( 6 a), Cl ( 6 b)) and fcSe 2[P 3 N 3 X 5] (X = F ( 7 a), Cl ( 7 b)) are attached to only one phosphorus atom, and spirocyclic 1,3-dichalcogena-2-phospha-[3]ferrocenophanes are formed. All new products have been characterized on the basis of their 1 H, 13 C and 31 P NMR as well as EI mass spectra. The molecular structures of 5 a , b and 6 a have been determined by x-ray structure analyses.
    Notes: Die Hexahalogen-cyclotriphosphazene, P3N3X6 (X = F (1 a), Cl (1 b)), reagieren mit Ferrocenol, FcOH, im Molverhältnis 1 : 1 unter Bildung der Ferrocenoxy-Derivate FcO[P3N3X5] (X = F (3 a), Cl (3 b)); der tetramere Ring P4N4Cl8 (2 b) bildet in analoger Weise FcO[P4N4Cl7] (4 b). 1,1′-Ferrocendiol, fc(OH)2, setzt sich mit P3N3X6 im Molverhältnis 1 : 1 zu fcO2[P3N3X4] (X = F (5 a), Cl (5 b)) um; nach der Röntgenstrukturanalyse ist der 1,1′-Ferrocendiolato-Rest in 5 a, b an zwei verschiedene Phosphoratome gebunden. Dagegen werden die 1,1′-Ferrocendithiolat- und 1,1′-Ferrocendiselenolat-Reste in fcS2[P3N3X4] (X = F (6 a), Cl (6 b)) bzw. fcSe2[P3N3X4] (X = F (7a), Cl (7 b)) jeweils nur an ein Phosphoratom angekoppelt, so daß spirocyclische 1,2-Dichalkogena-2-phospha[3]ferrocenophane entstehen. Alle neuen Produkte wurden anhand ihrer 1H-, 13C- und 31P-NMR-Spektren und der EI-Massenspektren charakterisiert; für 5 a, b und 6 a wurde die Molekülstruktur durch Röntgenstrukturanalyse bestimmt.
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  • 26
    ISSN: 0044-2313
    Keywords: Octaisopropylmanganocene ; Hexa(tert.-butyl)-manganocene ; 1,1′,2,2′,4,4′-Hexaisopropyl-3,3′,5,5′-tetramethyl-manganocene ; 1,1′-Diisopropyl-octamethylmanganocene ; high spin complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: High Spin-Manganocenes with Bulky, Alkylated Cyclopentadienyl LigandsOctaisopropylmanganocene and hexa(tert.-butyl)manganocene show high spin behaviour whereas 1,1′,2,2′,4,4′-hexaisopropyl-3,3′,5,5′-tetramethylmanganocene exhibits spin crossover from high spin to low spin configuration on cooling below -106°C. 1,1′-Diisopropyl-octamethyl-manganocene is low spin at 36°C in solution. The electronic influence of ring alkylation favouring low spin manganocenes is superseded by the steric effect of metal-ring expansion weakening the ligand field and evoking high spin behaviour.
    Notes: Octaisopropylmanganocen und Hexa(tert.-butyl)manganocen zeigen high spin-Verhalten, während beim 1,1′,2,2′,4,4′-Hexaisopropyl-3,3′,5,5′-tetramethylmanganocen ein spin crossover von der high spin- zur low spin-Konfiguration beim Abkühlen unter -106°C auftritt. 1,1′-Diisopropyl-octamethylmanganocen zeigt low spin-Verhalten bei 36°C in Lösung. Der elektronische Einfluß der Ringalkylierung, welcher low spin-Manganocene begünstigt, wird bei Derivaten mit mehreren sperrigen Alkylgruppen übertroffen von einem sterischen Effekt der Metall/Ring-Abstandsvergrößerung, welche das Ligandenfeld schwächt und high spin-Verhalten hervorruft.
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  • 27
    ISSN: 0044-2313
    Keywords: Structure determination ; vanadium weberites ; disodium metal(II) vanadium(III) heptafluorides ; sodium tetrafluoro-vanadate(III) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of the Vanadium Weberites Na2MIIVIIIF7 (MII = Mn, Ni, Cu) and of NaVF4At single crystals of the vanadium(III) compounds NaVF4 (a = 790.1, b = 531.7, c = 754.0 pm, β = 101.7°; P21/c, Z = 4), Na2NiVF7 (a = 726.0, b = 1031.9, c = 744.6 pm; Imma, Z = 4) and Na2CuVF7 (a = 717.6, b = 1043.5, c = 754.6 pm; Pmnb, Z = 4) X-ray structure determinations were performed, at Na2MnVF7 (a = 746.7, c = 1821.6 pm; P3221, Z = 6) a new refinement. NaVF4 crystallizes in the layer structure type of NaNbO2F2. The fluorides Na2MIIVF7 represent new orthorhombic (MII = Ni; Cu) resp. trigonal (MII = Mn) weberites. The average distances within the [VF6] octahedra of the four compounds are in good agreement with each other and with data of related fluorides (V—F: 193.3 pm). The differences between mean bond lengths of terminal and bridging F ligands are 5% in NaVF4, but less than 1% in the weberites. Details and data for comparison are discussed.
    Notes: An Einkristallen der Vanadium(III)-Verbindungen NaVF4 (a = 790,1, b = 531,7, c = 754,0 pm, β = 101,7°; P21/c, Z = 4), Na2NiVF7 (a = 726,0, b = 1031,9, c = 744,6 pm; Imma, Z = 4) und Na2CuVF7 (a = 717,6, b = 1043,5, c = 754,6 pm; Pmnb, Z = 4) wurden Röntgenstrukturbestimmungen durchgeführt, an Na2MnVF7 (a = 746,7, c = 1821,6 pm; P3221, Z = 6) eine neue Verfeinerung. NaVF4 kristallisiert in der Schichtstruktur des NaNbO2F2-Typs. Die Fluoride Na2MIIVF7 sind neue orthorhombische (MII = Ni; Cu) bzw. trigonale (MII = Mn) Weberit-Vertreter. Die mittleren Abstände in den [VF6]-Oktaedern der vier Verbindungen stimmen gut miteinander und mit Daten in verwandten Fluoriden überein (V—F: 193,3 pm). Die Unterschiede zwischen den mittleren Abständen terminaler und verbrückender F-Liganden betragen in NaVF4 5%, in den Weberiten aber weniger als 1%. Einzelheiten und Vergleichsdaten werden diskutiert.
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  • 28
    ISSN: 0044-2313
    Keywords: Sodium auride thallide ; gold chains ; thallium dumb-bells, synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na4AuTl, the First Ternary Compound in the System Sodium/Gold/ThalliumSilver coloured, brittle single crystals of Na4AuTl were obtained by the reaction of NaN3, gold sponge and TlN3 at 773 K. The structure was determined from X-ray single-crystal diffractometry data: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm space}\,{\rm group}\,{\rm Fmmm,}\,{\rm Z = 8,}\,{\rm a = 5}{\rm .453(1)}\mathop {\rm A}\limits^ \circ,\,{\rm b = 10}{\rm .006(2)}\,\,\mathop {\rm A}\limits^ \circ,\,{\rm c = 23}{\rm .387(5)}\,\mathop {\rm A}\limits^ \circ $$\end{document} Na4AuTl crystallizes in a new structure type with separated gold and thallium partial structures. These consist of linear ∞1[Au2/2] chains and [Tl2] dumb-bells. Structural relationships between Na2Au and the Na Au partial structure of Na4AuTl are discussed.
    Notes: Silberfarbene, spröde Einkristalle eines bislang unbekannten Na4AuTl wurden durch Umsetzung von NaN3, Goldschwamm und TlN3 bei 773 K erhalten. Die Struktur wurde aus Röntgen-Einkristall-Diffraktometerdaten bestimmt: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm Raumgruppe}\,{\rm Fmmm,}\,{\rm Z = 8,}\,{\rm a = 5,453(1)}\mathop {\rm A}\limits^ \circ,\,{\rm b = 10,006(2)}\,\,\mathop {\rm A}\limits^ \circ,\,{\rm c = 23,387(5)}\,\mathop {\rm A}\limits^ \circ $$\end{document} Na4AuTl kristallisiert in einem neuen Strukturtyp mit voneinander separierten Gold- und Thallium-Teilstrukturen, die aus linearen ∞1[Au2/2]-Ketten und [Tl2]-Hanteln aufgebaut sind. Strukturbeziehungen zwischen Na2Au und der Na—Au-Teilstruktur von Na4AuTl werden diskutiert.
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  • 29
    ISSN: 0044-2313
    Keywords: Sodium trifluormethanesulfonate ; monohydrate ; crystal structure ; phase transition ; sodium ionic conduction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Sodium Trifluormethanesulfonate - Crystal Structure and Phase Transition of Sodium Trifluormethanesulfonate Monohydrate and Sodium Ion Conductivity of Anhydrous Sodium TrifluormethanesulfonateAccording to the results of temperature dependent powder diffractometry (Guinier-Simon-technique) sodium trifluormethanesulfonate monohydrate is dimorphous. The phase transition occurs at -35°C. The room-temperature modification crystallizes monoclinic in space group P21/c with the lattice parameters a = 941.6(5) pm, b = 654.3(2) pm, c = 1062.4(5) pm and β = 107.73(2)°. The crystal structure consists of double layers of trifluormethanesulfonate anions, the lipophilic CF3-groups pointing at each other. Sodium is coordinated by four oxygen atoms from four different anions and by two molecules of crystal water. The resulting polyhedron may be addressed as a distorted octahedron. The low-temperature modification crystallizes orthorhombic in space group Pnma with the lattice parameters a = 645.31(9) pm, b = 538.03(9) pm, c = 1745.3(3) pm. The loss of crystal water occurs at 136°C. Anhydrous sodium trifluormethanesulfonate shows a phase transition at 252°C. The high-temperature modification is a good sodium ionic conductor (σ = 4.1 · 10-1 Ω-1 cm-1 at 250°C).
    Notes: Nach Kühl-Guinier-Simon-Untersuchungen ist Natriumtrifluormethylsulfonatmonohydrat dimorph. Die Phasenumwandlung erfolgt bei -35°C. Die Raumtemperaturmodifikation kristallisiert monoklin in der Raumgruppe P21/c mit den Gitterkonstanten a = 941,6(5) pm, b = 654,3(2) pm, c = 1062,4(5) pm und β = 107,73(2)°. In der Kristallstruktur liegen Doppelschichten aus Trifluormethylsulfonatanionen vor, in denen die unpolaren CF3-Gruppen einander zugewandt sind. Natrium wird von jeweils einem Sauerstoffatom aus vier verschiedenen Anionen sowie von zwei Kristallwassermolekülen koordiniert und erreicht eine verzerrt oktaedrische Koordination. Die Tieftemperaturmodifikation kristallisiert orthorhombisch in der Raumgruppe Pnma mit den Gitterkonstanten a = 645,31(9) pm, b = 538,03(9) pm, c = 1745,3(3) pm. Die Abgabe von einem Mol Kristallwasser erfolgt bei 136°C. Wasserfreies Natriumtrifluormethylsulfonat zeigt eine Phasenumwandlung in eine Hochtemperaturmodifikation bei 252°C, die eine gute Natriumionenleitfähigkeit zeigt (σ = 4,1 · 10-1 Ω-1 cm-1 bei 250°C).
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  • 30
    ISSN: 0044-2313
    Keywords: (CH3)2S derivatives ; Structure ; Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (CH3)2SBr2 - Reactions and Structures(CH3)2SBr2 (1) is a donor acceptor complex (8-S-3 + 10-Br-2) which reacts with (CH3)2S(=O)NSi(CH3)3 to yield [(CH3)2S(O)=N—S(CH3)2]+Br- (2). With SbBr3 (CH3)2SBr+SbBr4- (3) can be isolated. 1 crystallizes monoclinic in the space group P21/c with a = 733.8, b = 734.2, c = 1132.7 pm, β = 92.8° and Z = 4. 2 crystallizes in the orthorhombic space group Pnma with a = 967.2, b = 793.3, c = 1168.3 pm and Z = 4. The SBr and BrBr force constants of 1 are compared with those of S2Br2, 3 and Br2 resp. The nmr and mass spectra of 1 and 2 are communicated.
    Notes: (CH3)2SBr2 (1) ist ein (8-S-3 + 10-Br-2) Donor-Akzeptor-Komplex(8-S-3 + 10-Br-2) bedeutet: acht Valenzelektronen am S-Atom, das von drei Bindungspartnern umgeben ist, und zehn Valenzelektronen am Br-Atom, das zwei Bindungspartner hat; s.: S. W. Perkins, J. C. Martin, A. J. Arduengeo III, W. Lau, A. Alegria, J. K. Kochi, J. Am. Chem. Soc. 1980, 102, 7753. und reagiert mit (CH3)2S(=O)NSi(CH3)3 zu [(CH3)2S(O)=N—S(CH3)2]+Br- (2), mit SbBr3 zu (CH3)2SBr+SbBr4- (3). 1 kristallisiert monoklin (P21/c) mit a = 733,8, b = 734,2, c = 1132,7 pm, β = 92,8° und Z = 4. 2 kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 967,2, b = 793,3, c = 1168,3 pm und Z = 4. Die SBr- und BrBr-Kraftkonstanten von 1 werden mit denen von S2Br2 und 3 bzw. Br2 verglichen. Die NMR- und Massenspektren von 1 und 2 werden kurz diskutiert.
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  • 31
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1639-1643 
    ISSN: 0044-2313
    Keywords: Lanthanoide chalcogenidehalides ; erbium selenidebromide ; erbium selenideiodide ; sodium erbium selenide ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of ErSeI and NaErSe2It is reported about attempts to synthesize lanthanoide selenidehalides of the formula LnSeX (X = Cl, Br, I) exemplary for Ln = Er. The relative stabilities of these compounds are discussed. X-ray crystal structure analysis revealed for the compounds ErSeBr and ErSeI the FeOCl-structure type (space group Pmmn, Z = 2, a = 406.3(5) pm, b = 559.2(6) pm, and c = 795(1) pm, and a = 418.26(6) pm, b = 558.4(1) pm, and c = 889.0(2) pm, respectively). A corresponding chloride was not found within the scope of this investigation. From the educts Er2Se3 and ErCl3 in the presence of NaCl as flux in Nb-ampoules the compound NaErSe2 was formed instead which crystallizes in an α-NaFeO2-type structure (space group R3m, Z = 3, a = 408.41(2) pm and c = 2067.4(2) pm).
    Notes: Berichtet wird über die Versuche zur Synthese von Lanthanoidselenidhalogeniden der Formel LnSeX (X = Cl, Br, I) am Beispiel Ln = Er. Die relativen Stabilitäten der angesprochenen Verbindungen untereinander werden diskutiert. Die Röntgenstrukturanalyse ergab für die Verbindungen ErSeBr und ErSeI den FeOCl-Strukturtyp (Raumgruppe Pmmn, Z = 2, a = 406.3(5) pm, b = 559.2(6) pm und c = 795(1) pm für X = Br und a = 418.26(6) pm, b = 558.4(1) pm und c = 889.0(2) pm für X = I). Ein entsprechendes Chlorid konnte im Rahmen dieser Untersuchungen nicht gefunden werden. Statt dessen bildete sich aus Er2Se3 und ErCl3 mit NaCl als Schmelzmittel in Nb-Ampullen die Verbindung NaErSe2, die im α-NaFeO2-Typ kristallisiert (Raumgruppe R3m, Z = 3, a = 408.41(2) pm und c = 2067.4(2) pm).
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  • 32
    ISSN: 0044-2313
    Keywords: Iron(II) complexes ; Schiff's base ligands ; crystal structure ; magnetic properties ; Mössbauer spectra ; electrochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Iron(II) Complexes with tetra- and pentadentate N,S-Chelate Ligands. Crystal Structure of [Fe(GBMA)py] · py (GBMA2- = Glyoxal bis-(2-mercaptoanil))The complexes glyoxal-bis-(2-mercaptoanil)iron(II) [Fe(GBMA)], diacetyl-bis-(2-mercaptoanil)iron(II), [Fe(DBMA)] and o-phthalaldehyde-bis-(2-mercaptoanil)iron(II) [Fe(PhBMA)] have been synthesized by reaction of the corresponding protonated ligands with anhydrous iron(II)-acetate. Pyridine-2,6-dialdehyde-bis-(2-mercaptoanil)iron(II), [Fe(PyBMA)] was obtained by a template synthesis with pyridine-2,6-dialdehyde, 2-aminothiophenol and iron(II)-acetate. Recrystallizing the complexes [Fe(GBMA)] and [Fe(DBMA)] from pyridine afforded [Fe(GBMA)py] · py and [Fe(DBMA)py] · py. For all complexes the magnetic properties have been determined, and the Mössbauer spectra were recorded at 82 K. Compounds [Fe(GBMA)] and [Fe(DBMA)] show quasi reversible redox properties in the cyclovoltammogram, while for [Fe(PhBMA)] an irreversible oxidation was observed. [Fe(GBMA)py] · py crystallizes in the monoclinic space group P21 with a = 1288.7(1), b = 1242.63(5), c = 1396.0(1) pm, β = 98.24(1)°, and Z = 4. In the neutral complex the Fe atom has a square pyramidal coordination with the pyridine nitrogen atom in apical position. The basal plane is formed by two nitrogen and two sulfur atoms of the ligand GBMA2-. The iron is located 40 pm above the pyramidal base. Its average distances to the donor atoms of the GBMA ligand are Fe—N = 190 pm, and Fe—S = 222 pm, while the distance to the nitrogen atom of the coordinated pyridine molecule is 207 pm.
    Notes: Die Komplexe Glyoxal-bis-(2-mercaptoanil)eisen(II), [Fe(GBMA)], Diacetyl-bis-(2-mercaptoanil)eisen(II), [Fe(DBMA)] und o-Phthaldialdehyd-bis-(2-mercaptoanil)eisen(II), [Fe(PhBMA)] wurden durch direkte Umsetzung der entsprechenden protonierten Liganden mit wasserfreiem Eisen(II)-acetat dargestellt. Die Synthese von Pyridin-2,6-dialdehyd-bis-(2-mercaptoanil)eisen(II), [Fe(PyBMA)] erfolgte mit Hilfe einer Templatsynthese aus 2,6-Pyridindialdehyd, 2-Aminothiophenol und Eisen(II)-acetat. Durch Umkristallisieren in Pyridin wurden aus [Fe(GBMA)] und [Fe(DBMA)] die Verbindungen [Fe(GBMA)py] · py und [Fe(DBMA)py] · py erhalten. Von allen Komplexen wurden die magnetischen Eigenschaften bestimmt und die Mössbauer-Spektren bei 82 K registriert. [Fe(GBMA)] und [Fe(DBMA)] zeigen im Cyclovoltammogramm quasireversibles Redoxverhalten, während bei [Fe(PhBMA)] eine irreversible Oxidation beobachtet wird. [Fe(GBMA)py] · py kristallisiert monoklin in der Raumgruppe P21 mit a = 1288,7(1), b = 1242,63(5), c = 1396,0(1) pm, β = 98,24(1)° und Z = 4. Im Neutralkomplex ist das Fe-Atom quadratisch-pyramidal mit dem Pyridin-Stickstoffatom in apikaler Position koordiniert. Die Pyramidenbasis wird von den zwei Stickstoff- und Schwefelatomen des Liganden GBMA2- aufgespannt. Das Fe-Atom befindet sich 40 pm oberhalb der Pyramidenbasis. Die Abstände zu den Donoratomen des GBMA-Liganden betragen im Mittel Fe—N = 190 pm und Fe—S = 222 pm. Der Fe—N-Abstand zum Pyridinstickstoffatom liegt bei 207 pm.
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  • 33
    ISSN: 0044-2313
    Keywords: Palladium Complexes ; Platinum Complexes ; Crown Ether Complexes ; Hexachlorodipalladate(II) ; Hexachlorodiplatinate(II) ; X-ray Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Crown Ether Complexes of Potassium Hexachlorodipalladate(II) and -diplatinate(II)K2[MCl4] (M = Pd, Pt) reacts with an excess of crown ether 18-crown-6 in water to give the crown ether complexes of potassium hexachlorodipalladate(II) and -diplatinate(II) [K(18-cr-6)]2[M2Cl6] (M = Pd, 1; M = Pt, 3), respectively, and in methylene chloride to give those of potassium tetrachloropalladate(II) and -platinate(II) [K(18-cr-6)]2[MCl4] (1) (M = Pd, 2; M = Pt, 4), respectively. 1-4 are characterized by microanalysis, NMR (1H, 13C), and vibrational spectroscopy. The X-ray structure analyses of the isotypic complexes 1 (P21/c; a = 10,9678(8), b = 8,2991(7), c = 22,469(2) Å, β = 98,523(5)°; Z = 2) and 3 (P21/c; a = 10,934(3), b = 8.376(3), c = 22,410(5) Å, β = 98,77(3)°; Z = 2) reveal [M2Cl6]2- anions of nearly D2h symmetry and [K(18-cr-6)]+ cations, in which the distance of K+ to the mean plane of the crown ether defined by its six oxygen atoms amounts to 0,830(4) Å in 1 and 0,821(2) Å in 3, respectively. There are tight contacts between cations and anions (d(K-Cl): 3,341(2)/3,260(2) Å (1); 3,348(4)/3,259(4) Å (3)).
    Notes: K2[MCl4] (M = Pd, Pt) reagiert mit überschüssigem Kronenether 18-Krone-6 in Wasser zu den Kronenetherkomplexen von Kaliumhexachlorodipalladat(II) bzw. -diplatinat(II) [K(18-cr-6)]2[M2Cl6] (M = Pd, 1; M = Pt, 3) und in Methylenchlorid zu denen von Kaliumtetrachloropalladat(II) bzw. -platinat(II) [K(18-cr-6)]2[MCl4] (M = Pd, 2; M = Pt, 4). 1-4 sind durch Elementaranalyse sowie NMR-(1H, 13C) und schwingungsspektroskopisch charakterisiert. Die Röntgeneinkristallstrukturanalysen der beiden isotypen Komplexe 1 (P21/c; a = 10,9678(8), b = 8,2991(7), c = 22,469(2) Å, β = 98,523(5)°; Z = 2) und 3 (P21/c; a = 10,934(3), b = 8,376(3), c = 22,410(5) Å, β = 98,77(3)°; Z = 2) zeigen [M2Cl6]2--Anionen von nahezu D2h-Symmetrie und [K(18-cr-6)]+-Kationen, in denen K+ in 1 um 0,830(1) Å bzw. in 3 um 0,821(2) Å aus der durch die sechs Sauerstoffatome des Kronenethers definierten Ebene ausgelenkt ist. Zwischen Kationen und Anionen bestehen enge Kontakte (d(K—Cl): 3,341(2)/3,260(2) Å (1); 3,348(4)/3,259(4) Å (3)).
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  • 34
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1657-1660 
    ISSN: 0044-2313
    Keywords: Ruthenium ; chalcogenide ; chemical transport ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of the Low Temperature Modification of RuTe2Black shining, platelet like single crystals of α-RuTe2 were obtained by chemical transport reaction with Cl2/AlCl3 (crystal dimensions up to 1 mm). The crystal structure of this low temperature modification of α-RuTe2 hitherto only known from powder measurements, was redetermined at room temperature by single crystal X-ray diffraction on a four-circle diffractometer. α-RuTe2 crystallizes in the marcasit structure typ in the orthorhombic spacegroup Pnnm (No. 58) with the lattice constants a = 528.12(13), b = 639.43(19), c = 400.85(13) pm.
    Notes: Durch chemischen Transport mit dem Transportmittel Cl2/AlCl3 konnten schwarzglänzende, plattenartige Einkristalle von α-RuTe2 erhalten werden (Kantenlänge bis zu 1 mm). Die Kristallstruktur dieser bisher nur aus Pulverdaten bekannten Tieftemperaturmodifikation von RuTe2 wurde röntgenographisch an einem Einkristall auf einem Vierkreisdiffraktometer bei Raumtemperatur neu bestimmt. α-RuTe2 kristallisiert im Markasit-Strukturtyp in der orthorhombischen Raumgruppe Pnnm (Nr. 58) mit den Gitterkonstanten a = 528,12(13), b = 639,43(19), c = 400,85(13) pm.
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  • 35
    ISSN: 0044-2313
    Keywords: Organo molybdenum compounds ; oxo complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mesityl Oxo Molybdenum and Tungsten Compounds. I. Structure of LiMoO2Me2Mes(OEt2)2LiMoO2Me2Mes(OEt2)2 2 is prepared by literature method [2] from MoO2Mes2 1 and LiMe. Its x-ray structure and NMR-spectral data are presented. 2 adopts a dimer structure in which two [MoO2Me2Mes]- anions are linked via two bridging [Li(OEt2)2]+ cations bonded to the oxo ligands. The resulting [‥OMoOLi‥]2 ring is planar.
    Notes: Die Struktur der bekannten, aus MoO2Mes2 1 und LiMe dargestellten Verbindung LiMoO2Me2Mes(OEt2)2 2 [2] sowie ihre NMR-spektroskopischen Daten werden mitgeteilt. 2 bildet ein in der Raumgruppe P1 kristallisierendes Dimer durch Verknüpfung zweier [MoO2Me2Mes]--Anionen über Oxo-Liganden durch zwei Kationen [Li(OEt2)2]+. Der gebildete [‥OMoOLi‥]2- Achtring ist eben.
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  • 36
    ISSN: 0044-2313
    Keywords: Di-μ-hydroxo-bis[(dimesylamido)(1,10-phenanthroline)dimethyltin(IV)] ; formation ; X-ray structure ; heptacoordinated tin ; hydrogen bond motifs ; linkage isomerism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonylamines. LXXXVIII. Occurrence of Three Linkage-Isomeric Complex Molecules in One Crystal: Formation and Structure of the Dimeric Dioganyltin(IV) Hydroxide [Me2{(MeSO2)2N}(phen)Sn(μ-OH)]2Crystal of the title compound (triclinic, space group P1) were obtained from Me2Sn[N(SO2Me)2]2 and 1,10-phenanthroline by adventitious hydrolysis. The structure consists of four independent [Me2{(MeSO2)2N}(phen)Sn(OH)] moieties A, A′, B, B′ that are associated via four-membered [SnO(H)]2 rings to form two centrosymmetric homodimers AA, BB and one asymmetric heterodimer A′B′. The four crystallographically independent tin atoms attain moderately distorted pentagonalbipyramidal coordinations, the apical positions being occupied by the methyl groups and the equatorial sites by the oxygen atoms of the μ-OH groups, the nitrogen atoms of the bidentate phen ligand and one oxygen atom of the (MeSO2)2N⊖ anion. Each anion is further connected to the respective complex core through an Sn—O—H… A hydrogen bond, where the acceptor A is nitrogen in AA and the A′ fragment of A′B′, or oxygen in BB and the B′ fragment of A′B′. The distinct hydrogen bond motifs in the three linkageisomeric complex units originate from two essentially different conformations of the dimesylamide anions.
    Notes: Kristalle der Titelverbindung (triklin, Raumgruppe P1) entstanden durch unplanmäßige Hydrolyse bei der Umsetzung von Me2Sn[N(SO2Me)2]2 mit 1,10-Phenanthrolin. Die Struktur besteht aus vier unabhängigen [Me2{(MeSO2)2N}(phen)Sn(OH)]-Einheiten A, A′, B und B′, die über viergliedrige [SnO(H)]2-Ringe zu zwei inversionssymmetrischen Homodimeren AA und BB sowie einem asymmetrischen Heterodimer A′B′ assoziiert sind. Die vier kristallographisch unabhängigen Zinnatome erreichen mäßig verzerrte pentagonal-bipyramidale Koordinationen, wobei die apikalen Positionen von den Methylgruppen, die äquatorialen Lagen von den Sauerstoffatomen der μ-OH-Gruppen, den Stickstoffatomen des zweizähnigen phen-Liganden und einem Sauerstoffatom des (MeSO2)2N⊖-Anions eingenommen werden. Ferner ist jedes Anion über eine Wasserstoffbrücke des Type Sn—O—H… A an den zugehörigen Komplexrumpf gebunden; als Akzeptor A wirkt in AA und im A′-Fragment von A′B′ das Stickstoffatom, in BB und im B′-Fragment von A′B′ ein Sauerstoffatom des Anions. Die Ausbildung bindungsisomerer Komplexe über unterschiedliche Wasserstoffbrückenmotive ist letztlich auf zwei grundlegend differierende Konformationen der Dimesylamid-Anionen zurückzuführen.
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  • 37
    Electronic Resource
    Weinheim : Wiley-Blackwell
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 38
    ISSN: 0044-2313
    Keywords: Chromium(II)-orthophosphate ; crystal growth ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Beiträge zum thermischen Verhalten und zur Kristallchemie von wasserfreien Phosphaten. XIX. Tri-chrom(II)-bis-phosphat Cr3(PO4)2 (≙ Cr6(PO4)4) - Ein Übergangsmetall(II)- Orthophosphat mit neuem StrukturtypIntensiv blau-violette Kristalle des bislang unbekannten Tri-chrom(II)-bis-phosphats, Cr3(PO4)2, entstehen bei der Reduktion von CrPO4 mit Chrom oberhalb von 1050°C (evakuierte Quarzglasampullen, wenige mg NH4I oder I2 als Mineralisator). Die Kristallstruktur von Cr3(PO4)2 enthält sechs kristallographisch unabhängige Cr2+ in der Elementarzelle (P212121, Z = 8, a = 8,4849(10) Å, b = 10,3317(10) Å, c = 14,206(3) Å). Davon sind fünf in der ersten Koordinationssphäre von vier Sauerstoffatomen leicht verzerrt quadratisch-planar umgeben (1,96 Å ≤ d(Cr—O) ≤ 2.15 Å). Deren Koordination wird vervollständigt durch zwei bzw. drei weiter entfernte Sauerstoffatome (2,32 Å ≤ d(Cr—O) ≤ 3,21 Å). Das sechste Cr2+-Ion ist stark verzerrt oktaedrisch koordiniert (d(Cr—O): 1,97, 2,04, 2,15, 2,28, 2,29, 2,53 Å).Die vier kristallographisch unterschiedlichen [PO4]-Gruppen zeigen nur geringe Abweichungen von der Geometric eines idealen Tetraeders (1,51 Å ≤ d(P—O) ≤ 1,57 Å; 104,3° ≤ ∠(O—P—O) ≤ 114,4°).Für die Cr2+ wurde mit μexp = 4,28(2) μB (θP = -54,8(5) K) ein ungewöhnlich niedriges mittleres magnetische Moment gefunden.
    Notes: Deep blue-violet single crystals of hitherto unknown chromous orthophosphate have been obtained reducing CrPO4 by elemental Cr at temperatures above 1050°C in evacuated silica ampoules (NH4I or I2 as mineraliser). The complex structure of Cr3(PO4)2 (P212121, Z = 8, a = 8.4849(10) Å, b = 10.3317(10) Å, c = 14.206(2) Å) contains six crystallographically independent Cr2+ per unit cell. Five of them are coordinated by four oxygen atoms which form a distorted (roof shaped) square plane as first coordination sphere at interatomic distances 1.96 Å ≤ d(Cr—O) ≤ 2.15 Å. Their coordination is completed by additional oxygen atoms (2 or 3) at distances 2.32 Å ≤ d(Cr—O) ≤ 3.21 Å. The sixth Cr2+ shows six-fold octahedral coordination with strong radial distortion (d(Cr—O): 1.97, 2.04, 2.15, 2.28, 2.29, 2.53 Å).The four different [PO4] groups exhibit only minor deviations from ideal tetrahedral geometry (1.51 Å ≤ d(P—O) ≤ 1.57 Å, 104.3° ≤ ∠(O—P—O) ≤ 114.4°).An unusually low magnetic moment μexp = 4.28(2) μB (θP = -54.8(5) K) has been observed for Cr2+.
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  • 39
    ISSN: 0044-2313
    Keywords: Organoindium compounds ; chelate complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The 3-(N,N-Dimethylamino)prop-1-enyl Group as a Chelate Ligand in Indium OrganylsInBr3 reacts with Me2NCH2CH=CHMgCl (molar ratio 1 : 2) to form (Me2NCH2CH=CH)2InBr (1) as the first indium alkenyl compound with amino-functionalized alkenyl groups. The X-ray structure determination shows the formation of a chelate complex. 1 crystallizes in the orthorhombic space group Fddd with the unit cell parameters a = 14.904(2) Å, b = 17.140(1) Å and c = 21.035(2) Å. By reaction of Me2InBr with Me2NCH2CH=CHMgCl (molar ratio 1 : 1) (Me2NCH2CH=CH)InMe2 (2) is formed as a colorless, at room temperature liquid, monomeric compound. The n.m.r. and mass spectra are discussed.
    Notes: InBr3 reagiert mit Me2NCH2CH=CHMgCl (Molverhältnis 1 : 2) in Diethylether als Lösungsmittel zu (Me2NCH2CH=CH)2InBr (1), der ersten Indium-Alkenylverbindung mit aminofunktionalisierten Alkenylresten. Die Röntgenkristallstrukturanalyse zeigt das Vorliegen eines Chelatkomplexes an. 1 kristallisiert orthorhombisch in der Raumgruppe Fddd mit Z = 16, a = 14,904(2) Å, b = 17,1405(14) Å und c = 21,035(2) Å. Aus Me2InBr und Me2NCH2CH=CHMgCl (Molverhältnis 1 : 1) wurde (Me2NCH2CH=CH)InMe2 (2) als farblose, bei Raumtemperatur flüssige, monomere Verbindung erhalten. Die 1H- und 13C-NMR-Spektren sowie Massenspektren werden mitgeteilt.
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  • 40
    ISSN: 0044-2313
    Keywords: New oxides of divalent copper ; crystal structure ; MAPLE ; absorption spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structures, and Absorption Spectra of the New “Cupriosilicates”: K6[CuSi2O8] and Rb4[CuSi2O7]K6[CuSi2O8] and Rb4[CuSi2O7] were obtained by annealing intimate mixtures of K2O and Rb2O, respectively, CuO and SiO2 in sealed Ag cylinders at 500°C as transparent greenish-blue single crystals. The structure solution (IPDS-data Mo Kα; K6[CuSi2O8]: 1292 F2(hkl), R1 = 0.059; wR2 = 0.103 and Rb4[CuSi2O7]: 763 F2(hkl), R1 = 0.049; wR2 = 0.114) confirms the space group P1 for both compounds. K6[CuSi2O8]: a = 619.4(2); b = 665.5(2); c = 753.0(2) pm; α = 83.66(3); β = 87.71(3); γ = 70.19(3)°; Z = 1. Rb4[CuSi2O7]: a = 631.9(9); b = 707.5(10); c = 715.2(6) pm; α = 114.2(1); β = 100.7(1); γ = 107.9(1)°; Z = 1. The Madelung Part of the Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these calculated via Mean Effective Ionic Radii, MEFIR, are given. The absorption spectra of K6[CuSi2O8] and Rb4[CuSi2O7] are discussed in terms of the Angular Overlap Model, AOM.
    Notes: K6[CuSi2O8] und Rb4[CuSi2O7] wurden erstmals durch Tempern innig verriebener Gemenge aus K2O bzw. Rb2O, CuO und SiO2 in verschlossenen Ag-Zylindern bei 500°C in Form von transparenten blaugrünen Einkristallen erhalten. Die Strukturaufklärung (IPDS-Datensätze, Mo-Kα; K6[CuSi2O8]: 1292 F2(hkl), R1 = 0,059; wR2 = 0,103 und Rb4[CuSi2O7]: 763 F2(hkl), R1 = 0,049; wR2 = 0,114) belegt die Raumgruppe P1 für beide Verbindungen. K6[CuSi2O8]: a = 619,4(2); b = 665,5(2); c = 753,0(2) pm; α = 83,66(3); β = 87,71(3); γ = 70,19(3)°; Z = 1. Rb4[CuSi2O7]: a = 631,9(9); b = 707,5(10); c = 715,2(6) pm; α = 114,2(1); β = 100,7(1); γ = 107,9(1)°; Z = 1. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, aus Mittleren Fiktiven Ionenradien, MEFIR, erhalten, werden angegeben. Die Absorptionsspektren von K6[CuSi2O8] und Rb4[CuSi2O7] werden anhand des Angular-Overlap-Modells, AOM, diskutiert.
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  • 41
    ISSN: 0044-2313
    Keywords: Barium ; Copper ; Vanadyl Phosphate ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cu4O12 Groups Built of Square Planar CuO4 Polygones in the Barium Vanadyl Oxocuprate(II) Phosphate Ba(VO)Cu4(PO4)4Single crystals of Ba(VO)Cu4(PO4)4 have been prepared by solid state reactions just below the melting points of the reaction mixtures of BaP2O6, Cu3(PO4)2, CuO, V2O5 and V2O3 in evacuated closed quartz glas tubes. The compound crystallizes with tetragonal symmetry, Space group D42—P4212, a = 9.560(2), c = 7.160(2) Å, Z = 2. Special and new features of the crystal structure are to each other isolated Cu4O12 and (VO)(PO4)4 groups. The crystal chemistry of the Cu4O12 groups is discussed with respect to other compounds containing out of plane connected square planar MO4 polygones.
    Notes: Einkristalle von Ba(VO)Cu4(PO4)4 wurden mit Festkörperreaktionen dicht unterhalb des Schmelzpunktes des Reaktionsgemenges aus BaP2O6, Cu3(PO4)2, CuO, V2O5 und V2O3 in geschlossenen, evakuierten Quarzglasampullen dargestellt. Diese Verbindung kristallisiert tetragonal, Raumgruppe D42—P4212, mit a = 9,560(2), c = 7,160(2) Å, Z = 2. Besondere und neue Eigenschaften der Kristallstruktur sind zueinander isolierte Cu4O12- und (VO)(PO4)4-Gruppen. Die Kristallchemie der Cu4O12-Baugruppen wird mit Blick auf andere Verbindungen, die nicht in Ebenen verknüpfte MO4-Polygone aufweisen, diskutiert.
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  • 42
    ISSN: 0044-2313
    Keywords: Ternary metal selenides ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Alkali Seleno Bismuthates (III), with a Comment Regarding the Th3P4 Structure TypeThe synthesis and X-ray single crystal structure determination of the ternary selenides Rb3BiSe3, Cs3BiSe3, and RbK2BiSe3 are described. The compounds were synthesized via a reaction of Bi2O3 with the alkali carbonate in a selencharged hydrogen stream at 850°C. They crystallize in the Na3AsS3 structure type (space group P213). In the discussion of the structure, the aristotypic Th3P4 structure is included.
    Notes: Es wird über die Darstellung und Einkristallstrukturbestimmung der ternären Selenide Rb3BiSe3, Cs3BiSe3 und RbK2BiSe3 berichtet. Die Synthese gelingt durch Umsetzungen von Bi2O3 mit dem entsprechenden Alkalicarbonat in einem mit Selen beladenen Wasserstoffstrom bei 850°C. Die Verbindungen kristallisieren im Na3AsS3-Typ (Raumgruppe P213). In die Strukturdiskussion wird der Th3P4-Typ als Aristotyp mit einbezogen.
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  • 43
    ISSN: 0044-2313
    Keywords: Tetrafluoroaurates(III) ; single crystal investigation and structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of MII[AuF4]2 (MII = Cd, Hg)Cd[AuF4]2 and the isotypic compound Hg[AuF4]2, both are yellow, crystallize tetragonal in the space-group P4/mcc-D24h (No. 124) with a = 575.0/575.6 pm, c = 1034.8/1042.3 pm and Z = 2. The single-crystals were obtained by solid-state reactions in goldtubes.
    Notes: Cd[AuF4]2 und das dazu isotype Hg[AuF4]2, beide gelb, kristallisieren tetragonal in der Raumgruppe P4/mcc-D24h (Nr. 124) mit a = 575.0 bzw. 575.6 pm, c = 1034.8 bzw. 1042.3 pm und Z = 2. Die Darstellung der Einkristalle erfolgte durch Festkörperreaktion der binären Fluoride im Goldrohr.
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  • 44
    ISSN: 0044-2313
    Keywords: Lithium Niobium Chloride ; Niobium Cluster ; Synthesis ; Crystal Structure ; Lithium mobility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Struktur und Eigenschaften von LiNb6Cl15Schwarze Einkristalle von LiNb6Cl15 wurden aus Reaktionen von Nb-Pulver, NbCl5 und LiCl in verschweißten Niobrohren bei 850°C hergestellt. Die Schweratomstruktur von LiNb6Cl15 (Ia3d (Nr. 230), Z = 16, a = 2055.5(2) pm at 100 K, R(F) = 0.028, R(F2) = 0.053) ist mit der Struktur von Ta6Cl15 isotyp. Die [Nb6Cl12]2+-Cluster sind in der Struktur dreidimensional über drei zusätzliche Cla-a verbrückt. Diese verbrücken alle Ecken der Niobcluster, entsprechend der Schreibweise [Nb6Cl12iCl6/2a-a]- (die Nb—Cla-a—Nb-Bindungswinkel betragen 140°). Bei tiefen Temperaturen sind die Lithiumionen über ein Drittel von Lagen (48 f) fehlgeordnet und besetzen Hohlräume in verzerrten Chlorid-Tetraedern, die eine gemeinsame Kante teilen. Diese Positionen der Lithiumionen repräsentieren die engsten Stellen der unendlichen Kanäle in der Struktur, die von Chlorid gebildet werden. 7Li-NMR-Messungen zeigen oberhalb von 170 K eine deutliche Zunahme der Lithiumionenbeweglichkeit.
    Notes: Black single crystals of LiNb6Cl15 were obtained from reactions of Nb powder, NbCl5 and LiCl in sealed niobium tubes at 850°C. The heavy atom structure of LiNb6Cl15 (Ia3d (no. 230), Z = 16, a = 2055.5(2) pm at 100 K, R(F) = 0.028, R(F2) = 0.053) is isotypic with the structure of Ta6Cl15. The [Nb6Cl12]2+ clusters in the structure are three-dimensionally interconnected via three additional Cla-a. These bridge all vertices of niobium clusters, consistent with [Nb6Cl12iCl6/2a-a]- (the Nb—Cla-a—Nb angles are 140°). At low temperatures the lithium ions are disordered over one-third of sites (48 f), occupying cavities inside of two distorted corner-sharing tetrahedra of chloride. These positions for lithium represent the narrowest sections of infinite channels in the structure built up by chloride. An increased lithium ion mobility is obtained above 170 K by 7Li-NMR measurements.
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  • 45
    ISSN: 0044-2313
    Keywords: Ternary nickel phosphides ; strontium ; barium ; crystal structure ; phase transition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Polymorphism of SrNi2P2 and Crystal Structure of BaNi2P2SrNi2P2 and BaNi2P2 were prepared by heating mixtures of the elements and investigated by single crystal X-ray methods. The Sr compound at room temperature crystallizes in a superstructure of the ThCr2Si2 type (NT-phase; Immm; Z = 6; a = 3.951(2), b = 11.853(2), c = 10.432(2) Å), which is caused by displacements of the atoms from the ideal positions; the P—P distances are 2.45 and 3.28 Å. With increasing temperature at 45°C (ambient pressure) and increasing pressure at 4 kbar (room temperature) respectively the compound undergoes first order phase transitions and crystallizes after that in the undistorted ThCr2Si2 type (I4/mmm; Z = 2). While the P atoms of the high temperature phase (HT-SrNi2P2: a = 3.948(1), c = 10.677(3) Å; 100°C) are isolated from each other (dp p: 3.12 Å) they most probably form pairs in the high pressure phase (HD-SrNi2P2: a = 4.003(1), c = 9.761(2) Å; ca. 4 kbar). This will be discussed on the basis of band structure calculations. BaNi2P2 (a = 3.947(1), c = 11.820(1) Å) also crystallizes in the ThCr2Si2 type structure, the P—P distance is extended to 3.71 Å.
    Notes: SrNi2P2 und BaNi2P2 wurden durch Erhitzen entsprechender Elementgemenge dargestellt und röntgenographisch mit Einkristallmethoden untersucht. Die Sr-Verbindung kristallisiert bei Normaltemperatur in einer Überstruktur des ThCr2Si2-Typs (NT-SrNi2P2: Immm; Z = 6; a = 3,951(2), b = 11,853(2), c = 10,432(2) Å), die durch Auslenkung der Atome aus den idealen Positionen verursacht wird. Die P—P-Abstände längs [001] betragen 2,45 und 3,28 Å. Die Verbindung durchläuft mit steigender Temperatur bei 45°C (Normaldruck) sowie mit zunehmendem Druck bei ca. 4 kbar (Normaltemperatur) jeweils eine Phasenumwandlung 1. Ordnung und kristallisiert dann im unverzerrten ThCr2Si2-Strukturtyp (I4/mmm; Z = 2). Während bei der Hochtemperaturphase (HT-SrNi2P2: a = 3,948(1), c = 10,677(3) Å; 100°C) der P—P-Abstand längs [001] 3,12 Å beträgt, liegt er bei der Hochdruckphase (HD-SrNi2P2: a = 4,003(1), c = 9,761(2) Å; ca. 4 kbar) dem c/a-Verhältnis zufolge vermutlich bei 2,45 Å. Die Gründe für die Phasenumwandlungen werden an Hand der elektronischen Struktur diskutiert, BaNi2P2 (a = 3,947(1), c = 11,820(1) Å) kristallisiert ebenfalls im ThCr2Si2-Typ, der P—P-Abstand längs [001] ist hier auf 3,71 Å aufgeweitet.
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  • 46
    ISSN: 0044-2313
    Keywords: Tetrafluoroaurate(III) ; AgII-compounds ; single crystal investigation ; structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Silver(II) Tetrafluoroaurate(III) Ag[AuF4]2Intensive green single crystals of Ag[AuF4]2 can be obtained by heating up micro crystalline Ag[AuF4]2 in autoclaves (p(F2) ∼ 200 bar, T ∼ 400°C, t ∼ 14 d). It crystallizes monoclinic, space group P21/n — C2h5; (No. 14) with a = 522.3(1), b = 1101.3(3), c = 550.5(2) pm, β = 94.98(3), Z = 2 and is isotypic with Pd[AuF4]2.
    Notes: Durch Tempern mikrokristalliner Ag[AuF4]2-Proben im Autoklaven (p(F2) ∼ 200 bar, T ∼ 400°C, t ∼ 14 d) wurden leuchtend grüne Einkristalle von Ag[AuF4]2 erhalten. Die Verbindung kristallisiert monoklin, in der Raumgruppe P21/n — C2h5; (Nr. 14) mit a = 522.3(1), b = 1101.3(3), c = 550.5(2) pm, β = 94.98(3)°, Z = 2 und ist isotyp zu Pd[AuF4]2.
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  • 47
    ISSN: 0044-2313
    Keywords: Ternary sodium chlorides ; Holmium ; Erbium ; Phase diagrams ; Thermodynamic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Chlorides in the Systems NaCl/HoCl3 and NaCl/ErCl3Phase diagrams of the systems NaCl/HoCl3 and NaCl/ErCl3 were determined by means of DTA and high-temperature XRD. There exist compounds Na3LnCl6, NaLnCl4 (Ln = Ho, Er) and NaHo2Cl7. NaHoCl4 undergoes a phase transition at 374°C from the NaGdCl4- to the NaErCl4- type of structure. The thermodynamic functions for the formation of the compounds from NaCl and LnCl3 were determined by solution calorimetry and e.m.f. measurements in galvanic cells for solid electrolytes. The compounds NaLnCl4 are the most stable ones.
    Notes: Die Zustandsdiagramme der Systeme NaCl/HoCl3 und NaCl/ErCl3 wurden mittels DTA und Hochtemperatur-Guinieraufnahmen untersucht. Es existieren Verbindungen Na3LnCl6 und NaLnCl4 (Ln = Ho, Er) sowie NaHo2Cl7. NaHoCl4 wandelt sich bei 374° vom NaGdCl4- in den NaErCl4-Typ um. Mittels Lösungskalorimetrie und EMK-Messungen in galvanischen Feststoffzellen wurden die thermodynamischen Funktionen der ternären Chloride bezüglich der Bildung aus NaCl und LnCl3 bestimmt. Die Verbindungen NaLnCl4 weisen die größte Stabilität auf.
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  • 48
    ISSN: 0044-2313
    Keywords: Yttrium(III) ; samarium(II) ; benzyl complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Lanthanide Halides with Alkalibenzyl Compounds. Synthesis and Crystal Structures of [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)], [(tmeda)2SmBr(μ-Br)2Li(tmeda)] and [(dme)2SmBr(μ-Br)]2Alkali-benzyl compounds react via a metathesis reaction with lanthanide halides to benzyl complexes of the rare earths. Reaction of [(C6H5CH2)Li(tmeda)] with YBr3 leads to the complex [(tmeda)Y(C6H5CH2)2 (μ-Br)2Li(tmeda)] 1, in which Yttrium and lithium are linked via two bromide bridges. However, the reaction of [(C6H5CH2)Li(tmeda)] with SmBr3 in toluene/tmeda leads under reduction of the Sm ion to the compound [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. 2 reacts with DME to yield the dimeric compound [(dme)2SmBr(μ-Br)]2 3. The structures of 1-3 were determined by X-ray single crystal structure analysis:1:Space group P21/c, Z = 4, a = 829.5(6) pm, b = 1477.9(11) pm, c = 2575.0(10) pm, β = 92.03(6)°,2:Space group P21, Z = 2, a = 954,7(3) pm, b = 1338.5(6) pm, c = 1244.9(5) pm, β = 107.51(3)°,3:Space group P1, Z = 1, a = 797.2(7) pm, b = 818.3(7) pm, c = 1169.7(8) pm, α = 100.96(6)°, β = 92.03(6)°, γ = 91.75(7)°.
    Notes: Alkalibenzylverbindungen reagieren mit Lanthanoidhalogeniden unter Salzabspaltung zu Benzylkomplexen der Seltenen Erden. [(C6H5CH2)Li(tmeda)] bildet mit YBr3 den Komplex [(tmeda)(C6H5CH2)2Y(μ-Br)2Li(tmeda)] 1, in dem das Yttriumion mit Lithium über zwei Bromo-Brücken verknüpft ist. Bei der Reaktion von [(C6H5CH2)Li(tmeda)] mit SmBr3 in Toluol/TMEDA erfolgt hingegen unter Reduktion die Bildung von [(tmeda)2SmBr(μ-Br)2Li(tmeda)] 2. Diese Verbindung bildet mit DME den zweikernigen Komplex [(dme)2SmBr(μ-Br)]2 3. Die Strukturen von 1, 2 und 3 wurden durch Einkristallstrukturanalyse geklärt:1:Raumgruppe P21/c, Z = 4, a = 829,5(6) pm, b = 1477,9(11) pm, c = 2575,0(10) pm, β = 92,03(6)°,2:Raumgruppe P21, Z = 2, a = 954,7(3) pm, b = 1338,5(6) pm, c = 1244,9(5) pm, β = 107,51(3)°,3:Raumgruppe P1, Z = 1, a = 797,2(7) pm, b = 818,3(7) pm, c = 1169,7(8) pm, α = 100,96(6)°, β = 92,03(6)°, γ = 91,75(7)°.
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  • 49
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1535-1541 
    ISSN: 0044-2313
    Keywords: Bismuth platinum iodide ; subhalide ; crystal structure ; pseudo-symmetry ; stacking faults ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bi13Pt3I7: A Subiodide with a Pseudo-Symmetric Layer StructureThe reaction of PtI2 with Bi and BiI at 630 K yields black, lustrous, air insensitive crystals of the subiodide Bi13Pt3I7. The layered crystal structure (triclinic, C1, a = 1581.0(2) pm, b = 912.6(1) pm, c = 2149.6(6) pm, α = 90.03(2)°, β = 96.96(2)°, γ = 90.11(1)°, V = 3078.6 · 106 pm3) contains edge-sharing [PtBi8/2] cubes, which form nets of Kagomé type. Iodine atoms fill the hexagonal-prismatic voids therein. These ∞2[(PtBi8/2)3I] layers are alternately separated by layers of iodine atoms or ∞1[BiI4-] zigzag-chains. The marked pseudo-symmetry of the structure favours stacking faults, which cause streaks of diffuse scattering in the diffraction pattern.
    Notes: Aus der Reaktion von PtI2 mit Bi und BiI bei 630 K erhält man schwarze, metallisch glänzende und luftbeständige Kristalle des Subiodids Bi13Pt3I7. In der schichtartig aufgebauten Kristallstruktur (triklin, C1, a = 1581,0(2) pm, b = 912,6(1) pm, c = 2149,6(6) pm, α = 90,03(2)°, β = 96,96(2)°, γ = 90,11(1)°, V = 3078,6 · 106 pm3) liegen Kagomé-Netze aus kantenverknüpften [PtBi8/2]-Würfeln vor, deren hexagonal-prismatische Lücken mit Iodatomen gefüllt sind. Diese ∞2[(PtBi8/2)3I]-Schichten sind abwechselnd durch eine Lage von Iodatomen oder eine Schicht aus parallel angeordneten ∞1[BiI4-]-Zickzackketten getrennt. Die in der Struktur stark ausgeprägte Pseudosymmetrie begünstigt Stapelfehler, welche sich auch in diffusen Streifen im Beugungsbild äußern.
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  • 50
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1555-1560 
    ISSN: 0044-2313
    Keywords: Iodocuprate(I) ; [Cu2I4]2- ; tetraphenylphosphonium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zwei neue Modifikationen von [P(C6H5)4]2[Cu2I4]Bei der Reaktion von granuliertem Kupfer mit Iod und [P(C6H5)4]I in trockenem Aceton unter Stickstoffatmosphäre wurden Einkristalle von zwei neuen Modifikationen von [P(C6H5)4]2[Cu2I4] erhalten. Sie kristallisieren monoklin, Raumgruppe P21/n (Nr. 14), a = 11.550(6), b = 7.236 (2), c = 27.232 (13) Å, β = 98.13(3)°, V = 2253(2) Å3 und Z = 2 ([P(C6H5)4]2[Cu2I4]-C) bzw. Raumgruppe Cc (Nr. 9), a = 17.133(5), b = 15.941(5), c = 18.762(6) Å, β = 114.02(1)°, V = 4681(3) Å3 und Z = 4 ([P(C6H5)4]2[Cu2I4] -D). In diesen Verbindungen liegen dimere di-μ-iodo-diiodocuprat(I)-Einheiten vor, die planar (C) bzw. gewinkelt (D) sind.
    Notes: Single crystals of two new modifications of [P(C6H5)4]2[Cu2I4] were obtained by reaction of granulated copper with iodine and [P(C6H5)4]I in dry acetone under nitrogen atmosphere. They crystallise monoclinically, space group P21/n (No. 14), a = 11.550(6), b = 7.236(2), c = 27.232(13) Å, β = 98.13(3)°, V = 2253(2) Å3, and Z = 2 ([P(C6H5)4]2[Cu2I4]-C), and space group Cc (No. 9), a = 17.133(5), b = 15.941(5), c = 18.762 (6) Å, β = 114.02(1)°, V = 4681(3) Å3, and Z = 4 ([P(C6H5)4]2[Cu2I4]-D), respectively. In these compounds the [CuI2]- anions form dimers di-μ-iodo-diiodocuprate(I), which are either planar (C) or folded (D).
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  • 51
    ISSN: 0044-2313
    Keywords: β-Mannofuranose anions ; L-Threitolato ligands ; rac-Arabitolato ligands ; ferrates(III) ; ferric carbohydrate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polyol Metal Complexes. 25. rac-Mannose, rac-Arabitol and L-Threitol as Deprotonated Ligands in Ferrates(III)Ba2[Fe2(β-rac-ManfH-5)2] · 12H2O (1), Sr4[Fe4(rac-Arab1,2,3,5H-4)4(OH)2]CO3 · 33 H2O (2), and Ba2[Fe2(L-ThreH-4)2(OH)2] · 12.5 H2O (3) (Man = mannose, Arab = arabitol, Thre = threitol) have been crystallized from alkaline aqueous solution. Crystal structure analysis revealed dinuclear ferrate(III) ions for 1 and 3, the former being a Ci-symmetrical homoleptic ferric complex with pentadentate pentaanions derived from racemic β-mannofuranose. In 3, besides tetradentate L-threitolato ligands, there is one terminal hydroxo ligand at each ferric center. Hydroxo ligands are also present in the Ci-symmetrical hexaanions of 2, which are tetranuclear planar entities built up from four edge-sharing FeO6 octahedra. However arabitol is a pentitol, the tetraanionic ligands are only tetradentate for steric reasons.
    Notes: Ba2[Fe2(β-rac-ManƒH-5)2] · 12 H2O (1), Sr4[Fe4(rac-Arab1,2,3,5H-4)4(OH)2]CO3 · 33H2O (2) und Ba2[Fe2(L-ThreH-4)2(OH)2] · 12,5 H2O (3) (Man = Mannose, Arab = Arabit, Thre = Threit) wurden aus wäßrig-alkalischer Lösung kristallisiert. 1 und 3 enthalten Diferrat(III)-Tetraanionen, die sich im homoleptischen, Ci-symmetrischen Mannosekomplex 1 von fünffach deprotonierter β-rac-Mannofuranose ableiten, die als fünfzähniger Ligand vorliegt. In 3 tritt zu den vierzähnigen Tetraanionen des L-Threits an jedem Eisen(III)-Zentrum ein endständiger Hydroxoligand hinzu. Auch in 2 mit vierzähnigen rac-Arabit-Tetraanionen als Liganden wird oktaedrische Umgebung der FeIII-Zentren durch terminale Hydroxoliganden erreicht; mit dem als Folge seiner Konfiguration nur vierzähnigen Pentit wird ein ebenes Vierkern-Hexaanion durch Kantenverknüpfung von vier FeO6-Oktaedern aufgebaut.
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  • 52
    ISSN: 0044-2313
    Keywords: Formation of NH4[Ge(NH3)F5] ; structure ; ammonolysis ; ir spectrum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ammonolysis Reaction of (NH4)2GeF6. Synthesis and Structure of NH4[Ge(NH3)F5](NH4)2GeF6 reacts with ammonia to yield NH4[Ge(NH3)F5] at 280°C. The reaction path was elucidated by in situ time and temperature resolved X-ray powder diffraction. NH4[Ge(NH3)F5] crystallizes isostructurally to NH4[Si(NH3)F5] in the tetragonal space group P4/n (No. 85) with lattice constants a = 619.41(1) pm and c = 724.70(1) pm. The germanium atom is coordinated by five fluorine atoms and the nitrogen atom of the ammonia molecule. The ammonium cation is located on the Wyckoff position (2 a) in P4/n. The crystal structure is stabilized by extensive hydrogen bonding.
    Notes: (NH4)2GeF6 reagiert mit Ammoniak bei 280°C zu NH4[Ge(NH3)F5]. Der Reaktionsverlauf wurde in situ mit Hilfe der zeit- und temperaturaufgelösten Röntgenpulverdiffraktometrie verfolgt. Das so dargestellte NH4[Ge(NH3)F5] kristallisiert isostrukturell mit NH4[Si(NH3)F5] in der tetragonalen Raumgruppe P4/n (Nr. 85) mit den Gitterkonstanten a = 619,41(1) pm und c = 724,70(1) pm. Dabei ist das Germaniumatom verzerrt oktaedrisch von fünf Fluoratomen und dem Stickstoffatom des Ammoniakmoleküls koordiniert. Das Ammoniumion liegt auf der Tetraederpunktlage (2 a) in P4/n. Die Verbindung wird durch Wasserstoffbrückenbindungen stabilisiert.
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  • 53
    ISSN: 0044-2313
    Keywords: Barium ; platinum ; silicide ; gallium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Isotypic Compounds BaRh2Si2, BaIr2Si2, and BaPt2Ga2 - a Monoclinic Distortion Variant of the CaRh2B2 StructureThe new compounds BaRh2Si2 (monoclinic, P21/c, a = 792.6(1) pm, b = 664.5(7) pm, c = 767.9(4) pm, β = 91.2(1)°, Z = 4, 2867 reflexions, 47 parameters, R = 0.024), BaIr2Si2 (monoclinic, P21/c, a = 792.47(6) pm, b = 664.28(6) pm, c = 772.22(6) pm, β = 92.181(7)°, Z = 4, 1939 reflexions, 47 parameters, R = 0.037) and BaPt2Ga2 (monoclinic, P21/c, a = 850.4(1) pm, b = 647.3(1) pm, c = 819.8(1) pm, β = 95.97(1)°, Z = 4, 1506 reflexions, 47 parameters, R = 0.038) were prepared by reaction of the elements. Their structures were determined from single crystal data. The compounds crystallize isotypically with a distortion variant of the CaRh2B2 type of structure.
    Notes: Die neuen Verbindungen BaRh2Si2 (monoklin, P21/c, a = 792,6(1) pm, b = 664,5(7) pm, c = 767,9(4) pm, β = 91,2(1)°, Z = 4, 2867 Reflexe, 47 Parameter, R = 0,024), BaIr2Si2 (monoklin, P21/c, a = 792,47(6) pm, b = 664,28(6) pm, c = 772,22(6)pm, β = 92,181(7)°, Z = 4, 1939 Reflexe, 47 Parameter, R = 0,037) und BaPt2Ga2 (monoklin, P21/c, a = 850,4(1) pm, b = 647,3(1) pm, c = 819,8(1) pm, β = 95,97(1)°, Z = 4, 1506 Reflexe, 47 Parameter, R = 0,038) wurden durch Reaktion der Elemente dargestellt und ihre Strukturen mit Einkristalldaten bestimmt. Die Verbindungen kristallisieren isotyp in einer Verzerrungsvariante des CaRh2B2-Typs.
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  • 54
    ISSN: 0044-2313
    Keywords: Phosphoraneiminato Complexes ; Boron Compounds ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphoraneiminato Complexes of Boron. Syntheses and Crystal Structures of [BBr2(NPMe3)]2, [B2Br3(NPiPr3)2]Br, [B2(NPEt3)4]Br2, [B2Br2(NPPh3)3]BBr4 and [{B2(NMe2)2}2(NPEt3)2]ClThe bromoderivatives of the title compounds are prepared from the corresponding silylated phosphoraneimines Me3SiNPR3 and boron tribromide. The boron subcompound [{B2(NMe2)2}2(NPEt3)2]Cl2 derives from Me3SiNPEt3 and B2Cl2(NMe2)2. All complexes are characterized by NMR and IR spectroscopy as well as by crystal structure determinations.[BBr2(NPMe3)]2 (1): Space group P21/n, Z = 2, R = 0.031. Lattice dimensions at -50°C: a = 723.8, b = 894.2, c = 1305.4 pm, β = 92.35°. 1 forms centrosymmetric molecules in which the boron atoms are linked via μ2-N bridges of the NPMe3- groups of from B2N2 four-membered rings with B—N distances of 149.9 and 150.9 pm.B2Br3(NPiPr3)2]Br (2): Space group P21, Z = 2, R = 0.059. Lattice dimensions at -80°C: a = 817.6, b = 2198.7, c = 851.5 pm, β = 115.09°. In the cations of 2 the boron atoms are lined via the μ2-N atoms of the NPiPr3- groups to form planar, asymmetric B2N2 four-membered rings with B—N distances of 143 and 156 pm.[B2(NPEt3)4[Br2·4CH2Cl2 (3): Space group C2/c, Z = 4, R = 0.042. Lattice dimensions at -50°C: a = 1946.1, b = 1180.3, c = 2311.3 pm, β = 101.02°. The structure contains centrosymmetric dications in which both the boron atoms are lined by the N atoms of two of the NPEt3- groups to form a B2N2 four-membered ring with B—N distances of 149.6 pm. The remaining two NPEt3- groups are terminally bonded with very short B—N distances of 133.5 pm.B2Br2(NPPh3)3]BBr4 (4): Space group P1, Z = 2, R = 0.065. Lattice dimension at -50°C: a = 1025.7, b = 1496.1, c = 1807.0 pm, α = 85.09°, β = 82.90°, γ = 82.72°. In the cation the boron atoms are lined via the μ2-N atoms of two of the NPPh3- groups to form a nearly planer B2N2 four-membered ring with B—N distances of 149.3-153.1 pm. The third NPPh33 group is terminally connected with teh sp2 hybridized boron atom and with a B—N distance of 134.1 pm along with an almost linear BNP bond angle of 173.6°.[{B2(NMe2)2}2(NPEt2)2]Cl2 · 3CH2Cl2 (5): Space group C2/c, Z = 4, R = 0.098. Lattice dimensions at -70°C: a = 1557.9, b = 1294.7, c = 2122.9 pm, β = 96.08°. The structure of 4 contains centrosymmetric dications in which two by two B-B dumb-bells are linked via the μ2-N atoms of the two NEPt3- groups to form B4N2 six-membered rings with B—N distances of 150 and 156 pm and B-B distances of 173 pm. The B—N distances of the terminally bonded NMe2- groups correspond to 138 pm double bonds.
    Notes: Die Bromoderivate der Titelverbindungen werden aus den entsprechenden silylierten Phosphaniminen Me3SiNPR3 und Bortribromid hergestellt. Die Borsubverbindung [{B2(NMe2)2}2(NPEt3)2]Cl2 entsteht aus Me3SiNPEt3 und B2Cl2(NMe2)2. Alle Komplexe werden durch NMR- und IR-Spektren sowie durch Kristallstrukturanalysen charakterisiert.[BBr2(NPMe3)]2 (1): Raumgruppe P21/n, Z = 2, R = 0,031. Gitterkonstanten bei -50°C: a = 723,8; b = 894,2; c = 1305,4 pm; β = 92,35°. 1 bildet zentrosymmetrische Moleküle, in denen die Boratome über μ2-N-Brücken der NPMe3--Gruppen zu B2N2-Vierringen mit B—N-Abständen von 149,9 und 150,9 pm verknüpft sind.[B2Br3(NPiPr3)2]Br (2): Raumgruppe P21, Z = 2, R = 0,059. Gitterkonstanten bei -80°C: a = 817,6; b = 2198,7; c = 851,5 pm; β = 115,09°. In den Kationen von 2 sind die Boratome über die μ2-N-Atome der NPiPr3--Gruppen zu planaren, asymmetrischen B2N2-Vierringen mit B—N-Abständen von 143 und 156 pm verknüpft.[B2(NPEt3)4]Br2 · 4 CH2Cl2 (3): Raumgruppe C2/c, Z = 4, R = 0,042. Gitterkonstanten bei -50°C: a = 1946,1; b = 1180,3; c = 2311,3 pm; β = 101,02°. Die Struktur enthält zentrosymmetrische Dikationen, in denen die N-Atome zweier NPEt3--Gruppen die beiden Boratome zu einem B2N2-Vierring mit B—N-Abständen von 149,6 pm verknüpfen. Die beiden übrigen NPEt3--Gruppen sind terminal gebunden mit sehr kurzen B—N-Abständen von 133,5 pm.[B2Br2(NPPh3)3]BBr4 (4): Raumgruppe P1, Z = 2, R = 0,065. Gitterkonstanten bei -50°C: a = 1025,7; b = 1496,1; c = 1807,0 pm; α = 85,09°; β = 82,90°; γ = 82,72°. In dem Kation sind die Boratome über die μ2-N-Atome zweier NPPh3--Gruppen zu einem nahezu planaren B2N2-Vierring mit B—N-Abständen von 149,3-153,1 pm verknüpft. Die dritte NPPh3--Gruppe ist mit dem sp2-hybridisierten Boratom terminal mit einem B—N-Abständ von 134,1 pm verbunden bei einem fast linearen BNP-Bindungswinkel von 173,6°.[{B2(NMe2)2}2(NPEt3)2]Cl2 · 3 CH2Cl2 (5): Raumgruppe C2/c, Z = 4, R = 0,098. Gitterkonstanten bei -70°C: a = 1557,9; b = 1294,7; c = 2122,9 pm; β = 96,08°. Die Struktur von 4 enthält zentrosymmetrische Dikationen, in denen je zwei B—B-Hanteln über die μ2-N-Atome der beiden NPEt3--Gruppen zu B4N2-Sechsringen mit B—N-Abständen von 150 und 156 pm sowie B—B-Abständen von 173 pm verknüpft sind. Die B—N-Abstände der terminal gebundenen NMe2--Gruppen entsprechen mit 138 pm Doppelbindungen.
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  • 55
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 55-58 
    ISSN: 0044-2313
    Keywords: Tetrasodium triphosphate monohydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Na4HP3O10 · H2ONa4HP3O10 · H2O crystallizes orthorhombic in space group Pben with a = 693.2(5) pm, b = 1203.3(4) pm, c = 1188.5(4) pm; Z = 4. The obtained X-ray diffraction data (9268 symmetrical independent reflections, R = 0.047) allowed to locate and refine all the hydrogen atoms. The structure of Na4HP3O10 · H2O contains alternating layers of triphosphate anions and sodium cations. The triphosphate ions have site symmetry C2 and are linked by strong oxygen-hydrogen bonds (244 pm). The results of thermochemical analyses as well as the vibrational spectrum and data of 31P-MAS-NMR are submitted.
    Notes: Na4HP3O10 · H2O kristallisiert orthorhombisch in der Raumgruppe Pbcn mit a = 693,2(5) pm, b = 1203,3(4) pm, c = 1188,5(4) pm; Z = 4. Die erhaltenen Röntgenbeugungsdaten (9268 symmtrieunabhängige Reflexe, R = 0,047) ermöglichten die Lokalisierung und Verfeinerung sämtlicher Wasserstoffatome. Die Struktur von Na4HP3O10 · H2O besteht aus alternierenden Schichten von Triphosphatanionen und Natrium-Kationen. Die Triphosphationen weisen die Lagesymmetrie C2 auf und sind über starke Wasserstoffbrückenbindungen (244pm) miteinander verknüpft. Die Ergebnisse thermischer Analysen, sowie das Schwingungsspektrum und die 31P-MAS-NMR-Daten werden mitgeteilt.
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  • 56
    ISSN: 0044-2313
    Keywords: Hexanuclear tantalum chloro cluster ; tantalum cluster hydroxide ; mixed coordinated clusters ; intercluster bridges ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Kristallstrukturen von trans-[Ta6Cl12(OH)4(H2O)2] · 10 H2O und (NMe4)2[Ta6Cl12(OH)6] · 21 H2ODie Verbindungen trans-[Ta6Cl12(OH)4(H20)2] · 10H2O 1, (NMe4)2[Ta6Cl12(OH)6] · 21H2O 2 und Na2[Ta6Cll2(OH)6] · 16H2O 3 enthalten oktaedrische Tantalchlorocluster und können aus alkalischer Lösung (Methanol/Wasser) erhalten werden. Die Strukturen von 1 und 2 werden beschrieben. Kristallographische Daten s. Abstract.Die Verbindung 1 enthält neutrale, gemischt-koordinierte trans-[Ta6Cl12(OH)4(H2O)2]- Einheiten mit Ta—OH- und Ta—OH2Abständen von 210,4(5) und 214,5(5) pm. Ein koordiniertes Wassermolekül eines Clusters und eine OH Gruppe eines benachbarten Clusters bilden H3O2--Brücken mit einem O … H—O-Abstand von 253,7(7) pm zwischen den beiden Clustern aus. Die zwölf Ta—Cl-Abstände liegen zwischen 244,1(2) und 245,2(2) pm. Die Struktur von 2 ist aus [Ta6Cl12(OH)6]2--Anionen, NMe4+-Kationen und über H-Brücken gebundenen Wassermolekülen aufgebaut.
    Notes: The compounds trans-[Ta6Cl12(OH)4 (H2O)2] · 10 H2O 1, (NMe4)2[Ta6Cl12(OH)6] · 21 H2O 2 and Na2[Ta6Cl12(OH)6] · 16 H2O 3 containing octahedral tantalum chloro clusters were isolated from alkaline methanol/water solutions of [Ta6Cl12]4+. Crystal structures were solved for 1 and 2. Crystal data: 1, monoclinic, space group P21/c (No. 14), a = 938.5(2) pm, b = 1220.3(2) pm, c = 1391.7(4) pm, β = 103.87(2)°, V = 1547.5(6) × 106 pm3, Z = 2; 2, rhombohedral, space group R3 (No. 148), a = 1201.4(2) pm, c = 3110.8(6) pm, V = 3888.5(12) × 106 pm3, Z = 3; 3, cubic F lattice, a = 1451(2) pm, V = 3055(13) × 106 pm3, Z = 4.The cluster in 1 contains the neutral, mixed-coordinated trans-[Ta6Cl12(OH)4 (H2O)2] cluster with Ta—OH and Ta—OH2 distances of 210.4(5) pm and 214.5(5) pm, respectively. One coordinated H2O molecule from one cluster and a coordinated OH- group from a neighbouring cluster form H3O2- intercluster bridges with the O … H—O distance 253.7(7) pm. Twelve Ta—Cl (bridging) distances range from 244.1(2) to 245.2(2) pm. The structure of 2 is built of [Ta6Cl12(OH)6]2- anions, NMe4+ cations and water molecules, the latter linked to the anions by hydrogen bonds.
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  • 57