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  • Inorganic Chemistry  (83,670)
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  • 1
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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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  • 2
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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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  • 3
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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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  • 4
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    American Association for the Advancement of Science (AAAS)
    In: Science
    Publication Date: 2016-11-11
    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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  • 5
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    American Association for the Advancement of Science (AAAS)
    In: Science
    Publication Date: 2016-09-09
    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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  • 6
    Electronic Resource
    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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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1033-1034 
    ISSN: 0044-2313
    Keywords: Tetraphenylphosphonium-tetradecachlorotetraarsenate(III) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraphenylphosphonium Tetradecachlorotetraarsenate(III), (PPh4)2As4Cl14The title compound was obtained by reaction of As4S4, PPh4Cl and chlorine in dichloromethane. According to its X-ray crystal structure analysis, the As4Cl142- ion can be described as an association product of two AsCl4- units and two AsCl3 molecules. The As atoms and ten Cl atoms are approximately in a plane, the remaining four Cl atoms alternately take positions above and below this plane. The As atoms have distorted ψ octahedral coordination.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1040-1042 
    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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  • 9
    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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  • 10
    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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  • 11
    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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  • 12
    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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  • 13
    ISSN: 0044-2313
    Keywords: Structure determination ; [FeO5] square pyramide ; asymmetric [PbO6] coordination ; lone pair effect ; perovskite relation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Lead Strontium Ferrate(III): The Crystal Structure of the Phase Pb4Sr2Fe6O15At orthorhombic single crystals of Pb4Sr2Fe6O15 (a = 568.73(8), b = 392.03(4), c = 2107.5(3) pm; Z = 4/3, space group Pnma) a X-ray structure determination has been performed (R1 = 0,036 for 488 „observed“ resp. wR2 = 0,073 for all 643 independent reflexions). It revealed a framework of polyhedra related to perovskite, in which chains of edgesharing pyramids [FeO5] (average Fe1—O: 197 pm; Fe1—Fe1: 305.5 pm) are linked via apices with corner-sharing [FeO6] octahedra (Fe2—O: 201 pm). 12-fold, strongly distorted cuboctahedrally coordinated „perovskite positions“ show mixed occupancy by 2/3 Sr + 1/3 Pb (= Sr2; Sr2—O: 287 pm). More spacy channels, running parallel to the chains of pyramids along [010] of the structure, contain lead atoms only. The double occupancy of the corresponding cages results in short distances Pb1—Pb1 (355.9 pm) and Pb1—Fe2 (314.4 pm), as well as in a very asymmetric [PbO6] coordination (Pb1—O: 253 pm), in the opposite hemisphere of which the lone electron pair s2 is supposed to be located. Details are communicated and structural relations discussed.
    Notes: An orthorhombischen Einkristallen von Pb4Sr2Fe6O15 (a = 568,73(8), b = 392,03(4), c = 2107,5(3) pm; Z = 4/3, Raumgruppe Pnma) wurde eine Röntgenstrukturbestimmung durchgeführt (R1 = 0,036 für 488 „beobachtete“ bzw. wR2 = 0,073 für alle 643 unabhängigen Reflexe). Diese ergab ein perowskitverwandtes Polyedergerüst, in dem Ketten kantenverknüpfter [FeO5]-Pyramiden (Mittelwert Fe1—O: 197 pm; Fe1—Fe1: 305,5 pm) mit ihrerseits eckenverknüpften [FeO6]-Oktaedern (Fe2—O: 201 pm) über Ecken verbunden sind. Zwölffach, stark verzerrt kuboktaedrisch koordinierte „Perowskit-Positionen“ sind gemischt besetzt mit 2/3 Sr + 1/3 Pb (= Sr2; Sr2—O: 287 pm). Dagegen befinden sich in größeren Kanälen, die sich parallel zu den Pyramidenketten längs [010] durch die Struktur ziehen, nur Bleiatome. Die doppelte Besetzung der zugehörigen Hohlräume führt zu kurzen Abständen Pb1—Pb1 (355,9 pm) und Pb1—Fe2 (314,4 pm), und zu einer ganz einseitigen [PbO6]-Koordination (Pb1—O: 253 pm). in deren Gegenhemisphäre das s2-Elektronenpaar zu vermuten ist. Einzelheiten werden mitgeteilt und Strukturverwandtschaften diskutiert.
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  • 14
    ISSN: 0044-2313
    Keywords: Barium ; Cadmium ; Vanadium Oxide ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cadmium in Square Pyramids of Oxygen in the Barium Cadmium Oxovanadate: Ba2Cd3(VO4)2(V2O7)Single crystals of Ba2Cd3(VO4)2(V2O7) have been prepared by crystallization of a melt of BaCO3, CdO and V2O5. It shows orthorhombic symmetry, space group D42—P212121, a = 7.206(2), b = 9.978(1), c = 19.617(3) Å, Z = 4. The crystal structure is characterized by (VO4)3- and (V2O7)4- groups, CdO6 octahedra, BaO12 and BaO9 polyhedra and with respect to Cd containing oxides unusual square pyramids of O2- around Cd2+. The observed 1∞[CdO4] zickzack chains are connected by VO4 tetrahedra, V2O7 double tetrahedra and CdO5 pyramids, forming a tunnel structure along [100]. The tunnels are filled by barium.
    Notes: Einkristalle von Ba2Cd3(VO4)2(V2O7) wurden durch Kristallisation aus einer Schmelze von BaCO3, CdO und V2O5 dargestellt. Sie zeigen orthorhombische Symmetrie, Raumgruppe D42—P212121 mit a = 7,206(2), b = 9,978(1), c = 19,617(3) Å, Z = 4. Die Kristallstruktur zeichnet sich durch VO4-Tetraeder, V2O7-Tetraederdoppel, CdO6-Oktaeder, BaO12- und BaO9-Polyeder und für Cd unübliche tetragonale Pyramiden aus. Die beobachteten 1∞[CdO4]-Zick-zack-Ketten werden durch VO4-Tetraeder, V2O7-Tetraederdoppel und CdO5-Pyramiden unter Ausbildung einer längs [100] orientierten Tunnelstruktur vernetzt. Die Tunnel sind mit Ba2+ aufgefüllt.
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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: Pentachloromonocarbonylosmate(III) ; Crystalline Hydrate ; Crystal Structure ; Vibrational Spectra ; Normal Coordinate Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of K2[OsCl5(CO)] · H2OThe X-ray structure determination of K2[OsCl5(CO)] · H2O (monoclinic, space group P21/c a = 13.600(2), b = 7.122(1), c = 22.186(11) Å, β = 98.66(3)°, Z = 8) revealed two crystallographic independent bat very similar complex anions [OsCl5(CO)]2- with rough C4v point symmetry. Due to the stronger trans influence of the carbonyl group the bond lengths in the Cl—Os—CO axis Os—Cl = 2.449(2), 2.430(2) Å are langer as compared with the octahedron basis Os—Cl = 2.340-2.370 Å. The water of crystallization is coordinated to potassium (K—OH2 = 2.625-2.815 Å). Using the molecular parameters the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constants are fd(CO) = 15.30, fd(OsC) = 3.88, fd(OsCl) = 1.81, fd(OsCl) = 1.36, fd(OH) = 7.65, 7.82, 7.79 mdyn/Å. The strengthening of the Os—C bond by stronger back donation of the OsIII(d5) complex in comparison with the isostructural OsIV (d4) compound is discussed.
    Notes: Die Röntgenstrukturanalyse von K2[OsCl5(CO)] · H2O (monoklin, Raumgruppe P21/c a = 13,600(2), b = 7,122(1), c = 22,186(11) Å, β = 98,66(3)°, Z = 8) hat gezeigt, daß zwei kristallographisch unabhängige aber sehr ähnliche Komplexanionen [OsCl5(CO)]2- mit annähernd C4v-Punktsymmetrie vorliegen. Durch den größeren trans-Einfluß der Carbonylgruppe sind die Bindungsabstände in der Cl—Os—CO Achse Os—Cl = 2,449(2), 2,430(2) Å länger als in der Oktaederbasis: Os—Cl = 2,340-2,370 Å. Das Kristallwasser ist an Kalium koordiniert (K—OH2 = 2,625-2,815 Å). Mit den röntgenographisch bestimmten Molekülparametern lassen sich die IR- und Raman-Spektren durch Normalkoordinatenanalyse zuordnen. Die Valenzkraftkonstanten betragen fd(CO) = 15,30, fd(OsC) = 3,88, fd(OsCl) = 1,81, fd(OsCl) = 1,36, fd(OH) = 7,65, 7,82, 7,79 mdyn/Å. Die Festigung der Os—C-Bindung durch stärkere Rückbindung in dem OsIII(d5)-Komplex im Vergleich zur isostrukturellen OsIV(d4)-Verbindung wird diskutiert.
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  • 17
    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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  • 18
    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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  • 19
    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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  • 20
    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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  • 21
    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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  • 22
    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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  • 23
    Electronic Resource
    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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  • 24
    ISSN: 0044-2313
    Keywords: Zirconium ; Lithium ; Hydroxoligands ; Oxoligand ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Unusual Trimeric Bimetallic Li—Zr Complex with the Backbone [Zr3(μ2-OH)3(μ3-O)Li5] by Reaction of Zirconiumorgano and Hydrido Complexes with WaterThe reaction of compounds of the type [(LZr)(LiH)(L′)]n and [(LZr)(LiH)(L′)(alkyne)]n (L: 2,2′-Biphenolato-dianion, L′: thf, Bu3P, alkyne: Ph—C≡C—SiMe3, CH≡CH) with water at 0°C in a thf solution results in the formation of th trimeric bimetallic complex 8 [(L2Zr)3(μ2-OH)3(μ3-O)Li5(thf)8(H2O)5] in 50% yield. The X-ray analysis of 8 shows that a planar six-membered ring Zr3(μ2-OH)3 is formed. In the middle of this ring is a dianionic oxygen atom placed, coordinating to the three L2Zr centres in a planar μ3-coordination (bond angles 120,05μ). Five lithium ions stabilize the anionic backbone by bridging the biphenolato chelate ligands, which form seven-membered chelate rings with the atoms.1H-, 13C-, and 7Li-NMR spectra exhibit that the solid state structure remains unchanged in solution (thf).
    Notes: Die Reaktion von Verbindungen des Typs [(LZr)(LiH)(L′)]n und [(LZr)(LiH)(L′)(alkin)]n (L: 2,2′-Biphenolato-dianion, L′: thf, Bu3P, alkin: Ph—C≡C—SiMe3, CH≡CH) mit Wasser führt bei 0°C in thf in 50% Ausbeute zum trimeren Bimetallkomplex 8 [(L2Zr)3(μ2-OH)3(μ3-O) Li5(thf)8(H2O)5]. Die Kristallstrukturanalyse von 8 zeigt, daß ein planarer Zr3(μ2-OH)3-Sechsring gebildet wird. In seiner Mitte ist ein dianionisches Sauerstoffatom fixiert, das an den drei L2Zr-Zentren mit planarer μ3-Koordination gebunden ist (Bindungswinkel Zr—O—Zr 120,05°). Fünf Lithiumionen stabilisieren das anionische Gerüst durch Verbrückung der Biphenolatchelatliganden, die mit den Zr-Atomen Chelatsiebenringe ausbilden. 1H-, 13C- und 7Li-NMR-Spektren zeigen, daß in Lösung (thf) die Festkörperstruktur unverändert erhalten bleibt.
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  • 25
    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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  • 26
    ISSN: 0044-2313
    Keywords: Iridium ; ruthenium ; sodium ; calcium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturen und Charakterisierung von zwei neuen Oxiden vom Sr4PtO6-Typ: NaCa3IrO6 und NaCa3RuO6NaCa3IrO6 (I) und NaCa3RuO6 (II) kristallisieren mit trigonaler (rhomboedrischer) Symmetrie in der Raumgruppe R3c, Z = 6, I: a = 9,272(3) Å, c = 11,214(1) Å, II: a = 9,244(3) Å, c = 11,201(1) Å. I und II sind isotyp zu Verbindungen vom Sr4PtO6-Typ. Die Strukturen wurden mittels Röntgen-Einkristallstrukturanalyse gelöst mit einem R-Wert von 0,032 und Rw = 0,039 für I bzw. R = 0,024 und Rw = 0,031 für II. Die Struktur besteht aus unendlichen Ketten von flächenverknüpften MO6-Oktaedern mit M=Ir bzw. Ru und trigonalen Prismen von NaO6. Die Ketten sind getrennt durch Calcium-Kationen.
    Notes: NaCa3IrO6 (I) and NaCa3RuO6 (II) crystallize with trigonal (rhombohedral) symmetry in the space group R3c, Z = 6, for I a = 9.272(3) Å, c = 11.214(1) Å; for II a = 9.244(3) Å, c = 11.201(1) Å. NaCa3IrO6 (I) and NaCa3RuO6 (II) are isotypic to compounds of the Sr4PtO6 structure type. The structures have been solved by means of single crystal X-ray diffraction data analysis with the reliability factors for I of R = 0.032 and Rw = 0.039; and the the reliability factors for II of R = 0.024 and Rw = 0.031. The structure consists of infinite chains of alternating face-sharing MO6 octahedra, where M=Ir or Ru, and NaO6 trigonal prisms. The chains are separated by the calcium cations.
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  • 27
    ISSN: 0044-2313
    Keywords: Trihalogenogermane ; Germatrane ; Transmetalation ; Crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, Charakterisierung und Strukturen von 1-(9-Fluorenyl)germatran and 1-(Phenylacetylenyl)germatranÜber die Synthesen der Titelverbindungen, nämlich N(CH2CH2O)3GeY (2 Y=Fluorenyl; 4 Y=PhC≡C) durch Reaktion von X3GeY (1 Y=Fluorenyl, X=Br; 5 Y=PhC≡C, X=Cl) mit N(CH2CH2OSnR3)3 (3 R=Et; 6 R=Bu) wird berichtet und die Darstellung der neuen Verbindung 1 wird beschrieben. Die Strukturen der Verbindungen wurden durch Elementaranalysen sowie mittels 1H and 13C NMR-Spektroskopie bestimmt, 2 und 4 massenspektrometrisch charakterisiert. 1, 2 und 4 wurden mit Röntgenbeugungsmethoden analysiert.
    Notes: Syntheses of the title compounds, viz. N(CH2CH2O)3GeY (2 Y=Fluorenyl; 4 Y=PhC≡C) by the reaction of X3GeY (1 Y=Fluorenyl, X=Br; 5 Y=PhC≡C, X=Cl) with N(CH2CH2OSnR3)3 (3 R=Et; 6 R=Bu) are reported including the preparation of the new compound 1. Identity and structures were established by elemental analyses, 1H and 13C NMR spectroscopy. 2 and 4 were characterized by mass spectrometry. Single crystal structures of 1, 2 and 4 were determined by X-ray diffraction methods.
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  • 28
    ISSN: 0044-2313
    Keywords: Tetraalkyl phosphonium triiodide ; tetraalkyl arsonium triiodide ; tetraalkyl stibonium triiodide ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structure Analyses of Tetraalkyl Phosphonium, Arsonium, and Stibonium TriiodidesThe reaction of Me4EI (E=P, As), Me3EtSbI, Me2Et2SbI, MeEt3SbI, or Et4SbI with I2 in absence of solvent gives Me4PI3 (E=P, As), Me3EtSbI3, Me2Et2SbI3, MeEt3SbI3, or Et4SbI3. Me4SbI3 is formed in a reversible reaction by addition of I2 to (Me4Sb)3I8 or by reaction of a solution of Me4SbI in ethanol with I2 in benzene. The crystal structures of Me4EI3 (E=P, Sb), and Me3EtSbI3 and the syntheses of the novel compounds are reported.
    Notes: Die Reaktion von Me4EI (E=P, As), Me3EtSbI, Me2Et2SbI, MeEt3SbI oder Et4SbI mit I2 im Substanzgemisch ohne Lösungsmittel führt zu den entsprechenden Triiodiden Me4EI3 (E=P, As), Me3EtSbI3, Me2Et2SbI3, MeEt3SbI3 oder Et4SbI3. Me4SbI3 entsteht in reversibler Reaktion durch Zugabe von I2 zu (Me4Sb)3I8 oder durch Umsetzung einer ethanolischen Lösung von Me4SbI mit einer Lösung von Iod in Benzol. Über die Kristallstrukturen von Me4EI3 (E=P, Sb) und Me3EtSbI3 und die Synthese der neuen Verbindungen wird berichtet.
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  • 29
    ISSN: 0044-2313
    Keywords: Thia- and selena-arachno-undecaborane ; preparation ; spectroscopy ; ab initio/IGLO ; GIAO/NMR method ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thia- and Selena-arachno-undecaborane 6,7-μ-(CH3E)B10H13. Crystal Structure of arachno-6,7-μ-(CH3Se)B10H13. Theoretical Investigations of the Molecular Structures and 11B NMR Shifts of arachno-6,7-μ-(CH3E)B10H13The reaction of B10H14 with (CH3)2S yields with loss of H2 the base adduct 6,9-[(CH3)2S]2B10H12. Although an analogous reaction between B10H14 with disulfanes or diselenanes was expected to produce 6,9 bridged dichalcogen derivatives, (CH3)2S2 failed to react even under reflux conditions. Trisulfane (CH3)2S3 does react, but the pathway is different and leads to (CH3S)B10H13 2 without loss of H2. Unlike of (CH3)2S2, (CH3)2Se2 yields (CH3Se)B10H13, 3. Both 2 and 3 are formed by substitution of a bridging hydrogen and could be obtained in pure form and characterized 11B NMR spectroscopically. A single crystal X-ray structure analysis also was performed on 3 (space group P21/c). The molecular structures of 2 and 3 were optimized at the MP2 level and 11B NMR shifts were computed at the IGLO-SCF, GIAO-SCF and GIAO-B3LYP levels of theory.
    Notes: Bei der Reaktion zwischen B10H14 und (CH3)2S erfolgt unter H2-Abspaltung eine zweifache Adduktbildung, die zu 6,9-[(CH3)2S]2B10H12 führt. Die analoge Umsetzung zwischen B10H14 mit Disulfanen bzw. Diselenanen führte jedoch nicht zu den 6,9-Dichalkogen-verbrückten Derivaten. Bei der Umsetzung mit (CH3)2S2 findet selbst unter Refluxbedingungen keine Reaktion statt, wohl aber mit dem Trisulfan (CH3)2S3. Die Reaktion verläuft aber nicht unter H2-Abspaltung. Vielmehr wird dabei ein Brücken-H-Atom durch eine CH3S-Gruppe substituiert unter Bildung von (CH3S)B10H13 2. Im Gegensatz zu (CH3)2S2 findet aber mit (CH3)2Se2 ebenfalls eine Brücken-H-Substitution statt, wobei (CH3Se)B10H13 3 gebildet wird. 2 und 3 konnten in reiner Form isoliert und 11B-NMR-spektroskopisch charakterisiert werden. Von 3 wurde eine Röntgenstrukturanalyse durchgeführt (Raumgruppe P21/c) und von 2 und 3 die Molekülstrukturen auf MP2-Niveau optimiert sowie 11B-NMR- Verschiebungen mit IGLO-SCF, GIAO-SCF und GIAO-B3LYP berechnet.
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  • 30
    ISSN: 0044-2313
    Keywords: Titanium-Aluminium Alkoxide ; Aluminium Titanate (Tialite) ; Ceramics Precursor ; X-Ray Structure Determination ; 1H/13C-NMR (2 D) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structural Characterization of a Novel Titanium-Aluminium AlkoxideThe novel Ti-Al-Alkoxide TiAl2(OiPr)10, was synthesized from aluminium turnings and titanium tetraisopropoxide in 2-propanol and isolated by subsequent fractionating distillation. Colourless prismatic crystals precipitated after 24 h at 20°C from the main fraction. They proved very moisture sensitive. The compound crystallizes in the monoclinc space group C2/c (no. 15) with a = 2303.1(4), b = 1097.2(3), c = 1685.0(3) pm, β = 104.32(1)° and Z = 4. The molecular structure exhibits a bent Al-Ti-Al′ unit, in which Al shows tetrahedral, but Ti octahedral1 coordination. The polyhedra are connected via cis-edges of the octahedron. The structure of the compound in solution was determined by NMR spectroscopy (1H, 13C, COSY) and proved to be identical to the structure in the solid state.
    Notes: Das neue Ti-Al-Alkoxid TiAl2(OiPr)10 wurde durch Umsetzung von Al-Spänen mit Titantetraisopropoxid in Isopropanol und anschließender fraktionierender Destillation dargestellt. Die nach 24 h bei 20°C aus der Hauptfraktion gebildeten farblosen, prismatischen Kristalle sind sehr hydrolyseempfindlich. Die Kristallstruktur konnte bei -83°C bestimmt werden: monokline Raumgruppe C2/c (Nr. 15) mit a = 2303,1(4), b = 1097,2(3), c = 1685,0(3) pm, β = 104,32(1)° und Z = 4. Die Molekülstruktur besteht aus einer gewinkelten Al-Ti-Al′-Einheit, in der Al tetraedrisch und Ti oktaedrisch koordiniert sind. Die verknüpfenden Kanten am Ti-Oktaeder sind cis angeordnet. Die Struktur der Verbindung in Lösung wurde NMR-spektroskopisch (1H, 13C, COSY) ermittelt und stimmt mit der Struktur im Einkristall überein.
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  • 31
    ISSN: 0044-2313
    Keywords: Sulfoximide ; Sulfoximidium Salts ; Structure ; Hydrogenbonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfoximide and Sulfoximidium Salts - Structures and Hydrogen BondingIn the solid state dimethylsulfoximide (1) (orthorhombic; space group Pbca; a = 577.8, b = 931.2 and c = 1645.6 pm) makes intermolecular N—H ≡ N hydrogen bonds. The hydrogen halide salts (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reacts with metal halides to yield (CH3)2S(O)NH2+MHalyn- with the complex anions ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 crystallizes from ethanol (96%) as [(CH3)2S(O)NH2+Cl-]2 · H2O (3). The structures of 3 (monoclinic; space group P21/c; a = 917.0, b = 1344.7, c = 1080.8 pm and β = 103.8°; Z = 10), 4 (orthorhombic; space group Pbcn; a = 1028.9, b = 1132.6, c = 1074.1 pm; Z = 8) and 6 (monoclinic; space group C2/c; a = 2041.1, b = 1101.4, c = 3365.6 pm and β = 153.8°; Z = 8) are determined by X-ray analysis. In 6 Sb is coordinated in a distorted octahedra by 6 Cl in three short (mean 245,5 pm; SbCl3) and three long distances (291 to 299 pm; Cl-). Two of the chloride ions connect the Sb atoms to infinite Sb … Cl … Sb chains. Except for 7 and 9 there are bridges between the NH2 groups and the halide ions. The NH valence vibrations are discussed in view of hydrogen bonding.
    Notes: Im festen Dimethylsulfoximid (1) (orthorhombisch; Raumgruppe Pbca; a = 577,8, b = 931,2 und c = 1645,6 pm) sind zwischen den Imidgruppen N—H … N-Brückenbindungen ausgebildet. Die mit HHal darstellbaren Salze (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reagieren mit MHalx zu (CH3)2S(O)NH2+MHalyn- ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 kristallisiert aus 96% Ethanol als [(CH3)2S(O)NH2+Cl-]2 · H2O (3). Die Strukturen von 3 (monoklin; Raumgruppe P21/c; a = 917,0, b = 1344,7, c = 1080,8 pm und β = 103,8°; Z = 10), 4 (orthorhombisch; Raumgruppe Pbcn; a = 1028,9, b = 1132,6, c = 1074,1 pm; Z = 8) und 6 (monoklin; Raumgruppe C2/c; a = 2041,1, b = 1101,4, c = 3365.6 pm und β = 153,8°; Z = 8) wurden bestimmt. In 6 ist Sb verzerrt oktaedrisch von 6 Cl in drei kurzen (im Mittel 245,5 pm; SbCl3) und drei langen Abständen (291 bis 299 pm; Cl-) umgeben. Zwei der lang gebundenen Cl-Ionen verknüpfen die Sb-Atome zu unendlichen Sb … Cl … Sb-Ketten. Die NH2-Gruppen der Kationen bilden außer in 7 und in 9 H—Brückenbindungen zu den Halogenidionen. Die NH-Valenzschwingungen werden im Hinblick auf die Wasserstoffbrückenbindungen diskutiert.
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  • 32
    ISSN: 0044-2313
    Keywords: Copper(I) ; 1-azadienes ; oxidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Copper(I) Complexes with 1-Azadiene Chelate Ligands and Their Reaction with OxygenThe reaction of the bidendate 1-azadiene ligands Me2N—(CH2)n—N=CH—CH=CH—Ph with CuX results in the formation of the dimeric compounds [ACuX]2 and [BCuX]2 (A: n = 2, B: n = 3, X: I, Cl). The structure of complex 1 [ACuI]2 was determined by X-ray crystal structure analysis. 1 consists of two tetrahedrally coordinated Cu atoms connected by two iodo bridges. (Cu—Cu bond length: 261 pm).The ligand Me—N(CH2CH2N=CH—CH=CH—Ph)2 (C) reacts with CuX to form the monomeric complexes [CCuX] (5: X=I, 6: X=Cl). The crystal structure of 5 shows that the ligand acts as a tridendate ligand. The bond lengths of the CuN(sp2) bonds are significantly shorter than the Cu—N(sp3) distance.Reacting the podand-type ligands N(CH2CH2—N=CH—R)3 (D: R=Ph, E: R=-CH=CH—Ph) with CuX yields the ionic complexes 7 [DCu][CuCl2] and 8 [ECu][CuCl2]. 7 was characterized by X-ray analysis which confirmed that D acts as a four-dendate podand ligand.The compounds 1-8 are unreactive towards CO2 but take up O2 even at deep temperatures. At -78°C the orange-red complex 4 [BCuCl]2 reacts with O2 in CH2Cl2 to form a deep violet solution, but the primary product of the oxidation could not be isolated. It reacts at room temperature to form the green complex 9 [μ-Cl, μ-OH][BCuCl]2. The X-ray structure analysis of 9 confirms that a dimeric CuII complex is formed in which both a chloro- and a hydroxo group are bridging the monomeric units. The CuII centers exhibit a distorted tetragonal-pyramidal coordination.The pathway of the reaction with O2 will be discussed.
    Notes: Die Reaktion der zweizähligen 1-Azadienliganden Me2N—(CH2)n—N=CH—CH=CH—Ph mit CuX führt zu den dimeren Komplexen [ACuX]2 and [BCuX]2 (A: n = 2, B: n = 3, X: I, Cl). Die Struktur des Komplexes 1 [ACuI]2 wurde durch Kristallstrukturanalyse bestimmt. 1 enthält zwei tetraedrisch koordinierte Cu-Atome, die über zwei Iodobrücken miteinander verknüpft sind Cu—Cu-Bindungslänge: (261 pm).Der Ligand Me—N(CH2CH2N=CH—CH=CH—Ph)2 (C) reagiert mit CuX unter Bildung der monomeren Komplexe [CCuX] (5: X = I, 6: X=Cl). Die Kristallstruktur von 5 zeigt, daß der Ligand dreizählig koordiniert. Die Bindungslängen der Cu—N(sp2)-Bindungen sind signifikant kleiner als der Cu—N-(sp3)-Abstand.Die Reaktion der Podand-Liganden N(CH2CH2—N=CH—R)3 (D: R=Ph, E: R=-CH=CH—Ph) mit CuX führt zu den ionischen Komplexen 7 [DCu][CuCl2] bzw. 8 [ECu][CuCl2]. 7 wurde durch Röntgenstrukturanalyse charakterisiert, die ausweist, daß D als vierzähliger Ligand fungiert.Die Komplexe 1-8 sind gegenüber CO2 nicht reaktiv, nehmen aber O2 schon bei tiefen Temperaturen auf. Bei -78°C reagiert der orangerote Komplex 4 [BCuCl]2 mit O2 in CH2Cl2 zu einer tiefvioletten Lösung, das Primärprodukt der Oxidation konnte jedoch nicht isoliert werden. Es reagiert bei Raumtemperatur zu dem grünen Komplex 9 [μ-Cl, μ-OH][BCuCl]2. Die Kristallstrukturanalyse belegt, daß ein dimerer CuII-Komplex gebildet wird, in dem eine Chloro- und eine Hydroxobrücke die Monomereinheiten verbrücken. Die CuII-Zentren weisen eine verzerrt tetragonal-pyramidale Koordination auf.Der Reaktionsweg der Umsetzung mit O2 wird diskutiert.
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  • 33
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1190-1200 
    ISSN: 0044-2313
    Keywords: Phase investigation ; chemical transport reactions ; zinc molybdate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the System Zn/Mo/O. II. Chemical Transport of Ternary Zinc MolybdatesThe Chemical Transport is a method for preparation of phasepure multinary compounds with defined composition. We report about the possibilities to transport ternary compounds of the Zn/Mo/O system using Cl2, HCl, Br2, HBr, and I2 as an agent. The influence of the solid-gas equilibria on the compositions of solids, the transport direction, and the rate is showed.
    Notes: Der Chemische Transport ermöglicht eine gezielte phasenreine Darstellung von mehrkomponentigen Verbindungen mit definierter Zusammensetzung. Für das System Zn/Mo/O wird über die Möglichkeiten des Chemischen Transports der ternären Phasen mit den Transportmitteln Cl2, HCl, Br2, HBr und I2 berichtet. Dabei wird der Einfluß der Bodenkörper-Gasphase-Gleichgewichte auf die Bodenkörperzusammensetzungen, die Transportrichtung und Transportraten gezeigt.
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  • 34
    Electronic Resource
    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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  • 35
    ISSN: 0044-2313
    Keywords: Tris(perfluoroalkyl) arsenic and antimony ; tris(pentafluoroethyl) arsenic and antimony(V) halides ; synthesis ; NMR ; mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparations and Properties of Tris(perfluoroalkyl) Arsenic and Antimony(III, V) CompoundsAs(Rf)3 and Sb(Rf)3 (Rf=C2F5, C4F9, C6F13) are prepared in good yields by the polar reactions of AsCl3 and SbCl3 with bis(perfluoroalkyl) cadmium compounds as colourless liquids or solids. The oxidation of As(C2F5)3 and Sb(C2F5)3 with XeF2 gives the difluorides M(C2F5)3F2 (M=As, Sb). As(C2F5)3Cl2 is prepared by chlorination of As(C2F5)3 in the presence of AlCl3, while Sb(C2F5)3Cl2 is formed in the reaction of Sb(C2F5)3F2 with (CH3)3SiCl. During the reaction of M(C2F5)3F2 with (CH3)3SiBr 19F-NMR spectroscopic evidence is found for M(C2F5)3 Br2. The thermal decompositions of M(C2F5)3F2 mainly yield C4F10 and M(C2F5)F2, while the thermal decompositions of M(C2F5)3Cl2 yield M(C2F5)2Cl and C2F5Cl. The properties and spectroscopic data of the new compounds are described.
    Notes: As(Rf)3 und Sb(Rf)3 (Rf=C2F5, C4F9, C6F13) werden durch Umsetzungen von AsCl3 und SbCl3 mit Bis(perfluoralkyl)cadmium-Verbindungen unter polaren Bedingungen in guten Ausbeuten als farblose Flüssigkeiten bzw. Festkörper dargestellt. Durch Oxidation von As(C2F5)3 und Sb(C2F5)3 mit XeF2 entstehen die Difluoride M(C2F5)3F2 (M=As, Sb). Die Darstellung von As(C2F5)3Cl2 gelingt durch Chlorierung von As(C2F5)3 in Gegenwart von AlCl3; die Darstellung von Sb(C2F5)3Cl2 durch Reaktion von Sb(C2F5)3F2 mit (CH3)3SiCl. Die Dibromide M(C2F5)3Br2 sind nur 19F-NMR-spektroskopisch bei der Reaktion von M(C2F5)3F2 mit (CH3)3SiBr nachweisbar. Bei der thermischen Zersetzung von M(C2F5)3F2 entstehen hauptsächlich C4F10 und M(C2F5)F2, während die thermische Zersetzung von M(C2F5)3Cl2 unter Bildung von M(C2F5)2Cl und C2F5Cl verläuft. Eigenschaften und spektroskopische Daten der neuen Verbindungen werden beschrieben.
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  • 36
    ISSN: 0044-2313
    Keywords: Bis(dimesy1amido-O)tetraaquametal(II) complexes ; bis(dimesy1amido-O)tetrapyridinemetal(II) complexes ; synthesis ; X-ray structure; isotypic series ; Jahn-Teller distortion ; O—H…O, O—H…N and C—H…O hydrogen bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonylamines. LXXXIV. Isotypic Structures in the Dimesylamide Complex Series [M(H2O)4{(CH3SO2)2N}2] (M=Mg, Ca, Ni, Cu, Zn, Cd) and [M(py)4{(CH3SO2)2N}2] (M=Ni, Cu, Zn, Cd)The crystal structures of the trans-octahedral complexes [M(H2O)4{(CH3SO2)2N}2] (M=Ca, Cd), in which the dimesylamide anion acts as a monodentate O-ligand and a tetrafunctional hydrogen bond acceptor, were determined by low-temperature X-ray diffraction. Both belong to an isotypic series (triclinic, space group P1, Z = 1) that had previously been characterized for M=Mg, Ni, Cu and Zn (Z. Anorg. Allg. Chem. 1996, 622, 1065). In this structure there exists an extended network of strong hydrogen bonds which is probably the underlying reason why the structure type surprisingly persists across the whole series. To support this explanation by indirect evidence from comparison with suitable structures devoid of strong hydrogen bonding, the analogous trans-octahedral complexes [M(py)4{(CH3SO2)2N}2] (M=Mn, Co, Ni, Cu, Zn, Cd) were prepared by treating M[(CH3SO2)2N]2 with pyridine, and the crystal structures of the Ni, Cu, Zn and Cd compounds were studied by low-temperature X-ray crystallography. As anticipated, the four pyridine complexes do not form an isotypic series but instead two isotypic pairs consisting of the Ni and Zn compounds (monoclinic, space group P21/n, Z =2) and of the Cu and Cd complexes (triclinic, space group P1, Z = 1). All molecules of the aqua and the pyridine complexes display crystallographic centrosymmetry. In the hydrates, the mean M—OH2 and the M—O(anion) distances are 232.6 and 232.7 pm for M = Ca, 225.5 and 230.3 pm für M = Cd. The mean M—N and the M—O(anion) bond lengths of the pyridine species amount to 211.8 and 213.1 pm for M = Ni, 217.0 and 218.5 pm for M = Zn, 232.8 and 234.4 pm for M = Cd; the corresponding values for the severely Jahn-Teller distorted Cu complex are 203.6 and 254.5 pm. In the crystals of the pyridine complexes, each methyl group is connected through a weak C—H…O bond to a sulfonyl oxygen atom of an adjacent molecule.
    Notes: Die Kristallstrukturen der trans-oktaedrischen Komplexe [M(H2O)4{(CH3SO2)2N}2] (M=Ca, Cd), in denen das Dimesylamid-Anion als einzähniger O-Ligand und tetrafunktioneller Wasserstoffbrücken-Akzeptor wirkt, wurden durch Tieftemperatur-Röntgenbeugung ermittelt. Beide gehören zu einer isotypen Reihe (triklin, Raumgruppe P1, Z = 1), die zuvor für M=Mg, Ni, Cu und Zn charakterisiert worden war (Z. Anorg. Allg. Chem. 1996, 622, 1065). Hauptursache für die überraschende Persistenz der Isotypie in der gesamten Reihe ist vermutlich das in der Struktur auftretende hochorganisierte Netzwerk aus starken intermolekularen Wasserstoffbrücken. Um diese Annahme durch indirekte Evidenz an vergleichbaren Strukturen ohne starke H-Brücken zu überprüfen, wurden die analogen trans-oktaedrischen Komplexe [M(py)4{(CH3SO2)2N}2] (M=Mn, Co, Ni, Cu, Zn, Cd) aus M[(CH3SO2)2N]2 und Pyridin dargestellt und die Vertreter mit M=Ni, Cu, Zn und Cd durch Tieftemperatur-Röntgenbeugung untersucht. Der Erwartung entsprechend bilden die vier Pyridin-Komplexe keine isotype Reihe, aber zwei isotype Paare, die aus der Ni- und der Zn- Verbindung (monoklin, Raumgruppe P21/n, Z = 2) bzw, dem Cu- und dem Cd-Komplex (triklin, Raumgruppe P1, Z = 1) bestehen. Sämtliche Moleküle besitzen kristallographische Inversionssymmetrie. Die Mittelwerte der M—OH2- und die M—O(Anion)-Abstände in den Wasser-Komplexen betragen 232,6 und 232,7 pm für M=Ca, 225,5 und 230,3 pm für M=Cd. In den Pyridin-Komplexen sind die mittleren M—N- und die M—O(Anion)-Bindungslängen 211,8 und 213,1 pm für M=Ni, 217,0 und 218,5 pm für M=Zn, 232,8 und 234,4 pm für M=Cd sowie 203,6 und 254,5 pm für den eine erhebliche Jahn-Teller-Verzerrung aufweisenden Cu-Komplex. In den Kristallen der Pyridin-Komplexe ist jede Methylgruppe über eine schwache C—H … O-Wechselwirkung mit einem Sulfonyl-Sauerstoffatom eines Nachbarmoleküls verknüpft.
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  • 37
    ISSN: 0044-2313
    Keywords: Cobalt(II) complex ; 1,2-dimethyl-5-nitro-imidazole ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Crystal Structure of Bis(1,2-dimetyl-5-nitro-imidazole)dichlorocobalt(II)Bis(1,2-dimethyl-5-nitro-imidazol)dichlorocobalt(II) was obtained by reaction of CoCl2 · 6 H2O with 1,2-dimethyl-5-nitro-imidazole in methanol. The compound forms blue crystals which were characterized by IR and UV-vis spectroscopy and by an X-ray crystal structure determination. Co(C5H7N3O2)2Cl2: tetragonal, space group I42d, Z = 8, a = 1142.1(1) pm, c = 2577.3(2) pm. R = 0.036 for 670 independent reflexions. The Co atom is tetrahedrally surrounded by two chlorine and two N atoms at distances of 222.8(2) and 203.5(4) pm.
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  • 38
    ISSN: 0044-2313
    Keywords: Amine Alcohol Ligands ; Binuclear Complexes ; Gadolinium Complexes ; Magnetic Properties ; Schiff Base Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of a Binuclear Gadolinium(III) Complex: Magnetic Exchange Interactions in Alkoxy Bridged Lanthanide ComplexesThe Schiff Base ligand N-salicylidene-2-(bis-(2-hydroxyethyl)amino)ethylamine (H3sabhea) reacts with Gd(NO3)3 · 6 H2O in methanol solution to yield the alkoxy bridged binuclear gadolinium(III) complex [{Gd(Hsabhea)(NO3)}2] · 2MeOH (1). 1 crystallizes in the monoclinic space group P21/c with a = 1014.8(2), b = 2059.2(4), c = 867.5(2) pm, β = 106.72(2)°, and Z = 2. The two gadolinium atoms are bridged by two alkoxide oxygen atoms with angles of 107.60(11)° at the oxygen bridgeheads and a Gd—Gd separation of 376.43(7) pm. A variable-temperature magnetic susceptibility study (2 to 280 K) of 1 revealed an antiferromagnetic coupling between the Gd(III) ions with J = -0.198 cm-1 (g = 1.975).
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  • 39
    ISSN: 0044-2313
    Keywords: Ternary carbides ; crystal structure ; sodium ; palladium ; platinum ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Syntheses and Crystal Structures of Ternary Carbides Na2PdC2 and Na2PtC2Na2PdC2 and Na2PtC2 were synthesized by the reaction of sodium carbide with palladium and platinum respectively. The crystal structures could be solved from X-ray powder diffraction data (space group: P3m1, Z = 1). Both compounds crystallize in a new structure type with 1∞[M(C2)2/22-] chains (M≡Pd, Pt) as the characteristic structural unit. The existence of a C—C triple bond was confirmed by Raman spectroscopy.
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  • 40
    ISSN: 0044-2313
    Keywords: Sr3GdRhO6 ; Rietveld refinement ; magnetic susceptibility ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sr3GdRhO6 - die erste RhIII-Verbindung vom K4CdCl6-Strukturtyp: Synthese, Kristallstruktur und magnetische EigenschaftenSr3GdRhO6 wurde dargestellt und mittels Rietveld Verfeinerung von Röntgen-Pulverdaten (Raumgruppe R3c; Z = 6; a = 9,7840(5) Å; c = 11,4196(7) Å) charakterisiert. Diese Verbindung ist isostrukturell mit K4CdCl6 und die Struktur wird von unendlichen eindimensionalen Ketten von alternierend flächenverknüpften RhO6-Oktaedern und trigonalen Prismen von GdO6 aufgebaut. Die Strontium-Kationen sind in verzerrt-quadratisch-antiprismatischer Umgebung. Die Daten der magnetischen Suszeptibilität zeigen, daß Sr3GdRhO6 dem Curie'schen Gesetz gehorcht mit μ = 7,80 B.M. in Übereinstimmung mit der Oxidationsstufe +3 für Rhodium bzw. Gadolinium.
    Notes: The compound Sr3GdRhO6 has been synthesized and structurally characterized by Rietveld refinement of powder X-ray diffraction data. (space group R3c; Z = 6; a = 9.7840(5) Å; c = 11.4196(7) Å) This compound is isostructural with K4CdCl6. The structure consists of infinite one-dimensional chains of alternating face-shared RhO6 octahedra and GdO6 trigonal prisms. The strontium cations are located in a distorted square antiprismatic environment. Magnetic susceptibility data show that Sr3GdRhO6 obeys the Curie law with ηeff = 7.80 B.M., consistent with an oxidation state of +3 for both rhodium and gadolinium.
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  • 41
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1273-1276 
    ISSN: 0044-2313
    Keywords: Strontium tetrahydroxozincate monohydrate ; crystal structure refinement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of SrZn(OH)4 · H2OColorless crystals of SrZn(OH)4 · H2O are obtained by electrochemical oxidation of Zn in a zinc/iron pair in an aqueous ammonia solution saturated with strontium hydroxide. The X-ray crystal structure determination was now successful including all hydrogen positions: P1, Z = 2, a = 6.244(1) Å, b = 6.3000(8) Å, c = 7.701(1) Å, α = 90.59(1)°, β = 112.56(2)°, γ = 108.66(2)°, N(F2o ≥ 3σF2o) = 1967, N(Var.) = 84, R/Rw = 0.020/0.024.In SrZn(OH)4 · H2O Zn2+ is tetrahedrally coordinated by four OH- -ions while Sr2+ has 6 OH- and one H2O as neighbours. The polyhedra around Sr2+ are connected to chains which are linked three-dimensionally by isolated tetrahedra [Zn(OH)4]. Hydrogen bonds between H2O as donor and OH- are characterized by raman spectroscopy.
    Notes: Die elektrochemische Oxidation von Zink in einem Zink/Eisen Paar führt in einer wäßrigen ammoniakalischen Lösung von Strontiumhydroxid zu farblosen Kristallen von SrZn(OH)4 · H2O. An ihnen wurde röntgenographisch die Struktur jetzt einschließlich aller H-Lagen bestimmt: P1, Z = 2, a = 6,244(1) Å, b = 6,3000(8) Å, c = 7,701(1) Å, α = 90,59(1)°, β = 112,56(2)°, γ = 108,66(2)°, Z(F2o ≥ 3σF2o) = 1967, Z(Var.) = 84, R/Rw = 0,020/0,024.In SrZn(OH)4 · H2O ist Zn2+ tetraedrisch von OH- und Sr2+ von 6 OH- und einem H2O umgeben. Die Polyeder um Sr2+ bilden Ketten. Sie sind über isolierte Tetraeder [Zn(OH)4] dreidimensional verknüpft. Wasserstoffbrückenbindungen von H2O als Donator zu OH- sind durch Ramanspektroskopische Daten belegt.
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  • 42
    ISSN: 0044-2313
    Keywords: Silylenes ; 1,3-Diselena-2,4-disiletane ; 1,3-Ditellura-2,4-disiletane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silylene Reactions with Selenophene and a Tellurophene: Formation and Structures of a 1,3-Diselena-2,4-disiletane and a 1,3-Ditellura-2,4-disiletane [1]Di-tert-butylsilylene, generated by photolysis of hexa-tert-butylcyclotrisilane, reacts with selenophene or 2,5-dimethyltellurophene by chalcogen abstraction to furnish the 1,3-diselena-2,4-disiletane 6 and 1,3-ditellura-2,4-disiletane 7 ring systems. The X-ray structure analyses of 6 and 7 reveal strictly planar four-membered rings with the smaller endocyclic angles at the chalcogen and the larger angles at the silicon atoms.
    Notes: Photolytisch aus Hexa-tert-butylcyclotrisilan erzeugtes Di-tert-butylsilylen reagiert mit Selenophen oder 2,5-Dimethyltellurophen unter Chalkogenabstraktion zum 1,3-Diselena-2,4-disiletan 6 und 1,3-Ditellura-2,4-disiletan 7. Die Röntgenstrukturanalysen von 6 und 7 zeigen das Vorliegen planarer Vierringe mit den kleineren endocyclischen Winkeln an den Chalkogen- und den größeren an den Siliciumatomen.
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  • 43
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    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1287-1289 
    ISSN: 0044-2313
    Keywords: Calcium hexahydroxodizincate dihydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of CaZn2(OH)6 · 2 H2OThe electrochemical oxidation of zinc in a zinc/iron-pair leads in an aqueous NH3 solution of calciumhydroxide at room temperature to colourless crystals of CaZn2(OH)6 · 2 H2O. The X-ray structure determination was now successful including all hydrogen positions.P21/c, Z = 2, a = 6.372(1) Å, b = 10.940(2) Å, c = 5.749(2) Å, β = 101.94(2)° N(F2o ≥ 3σF2o) = 809, N(Var.) = 69, R/RW = 0.011/0.012The compound CaZn2(OH)6 · 2H2O contains Zn2+ in tetrahedral coordination by OH- and Ca2+ in octahedral coordination by four OH- and two H2O. The tetrahedra around Zn2+ form corner sharing chains, three-dimensionally linked by isolated polyhedra around Ca2+. Weak hydrogen bridge bonds result between H2O as donor and OH-.
    Notes: Die elektrochemische Oxidation von Zink in einem Zink/Eisen-Paar führt in einer wäßrigen NH3-Lösung von Calciumhydroxid bei Raumtemperatur zu farblosen Kristallen von CaZn2(OH)6 · 2 H2O. An ihnen wurde röntgenographisch die Struktur jetzt einschließlich aller H-Lagen bestimmt.P21/c, Z = 2, a = 6,372(1) Å, b = 10,940(2) Å, c = 5,749(2) Å, β = 101,94(2)° Z(F2o ≥ 3σF2o) = 809, Z(Var.) = 69, R/RW = 0,011/0,012In CaZn2(OH)6 · 2 H2O ist Zn2+ tetraedrisch von OH- und Ca2+ oktaedrisch von vier OH- und zwei H2O umgeben. Die Tetraeder um Zn2+ bilden Ketten über gemeinsame Ecken, die durch voneinander isolierten Oktaedern um Ca2+ dreidimensional verknüpft werden. Es liegen schwache H-Brückenbindungen von H2O als Donator zu OH- vor.
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  • 44
    ISSN: 0044-2313
    Keywords: Phosphorus(V) nitride imide ; deuterium compound of ; synthesis of ; x-ray, synchrotron and neutron structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystalline Phosphorus(V) Nitride Imide, HPN2 and DPN2, respectively, - Structure Determination with X-Ray, Synchrotron, and Neutron RadiationMicrocrystalline HPN2 resp. DPN2 was obtained by the reaction of P3N5 with NH3 resp. ND3 in high-pressure autoclaves under ammonothermal conditions (T = 550°C, p(NH3 resp. ND3) = 6 kbar) within 14 d.
    Notes: Mikrokristallines HPN2 bzw. DPN2 entsteht bei der Umsetzung von P3N5 mit NH3 bzw. ND3 in Hochdruckautoklaven unter ammonothermalen Bedingungen (T = 550°C, p(NH3 bzw. ND3) = 6 kbar) innerhalb von 14 Tagen.Die Struktur wurde an DPN2 über Beugungsexperimente mit Synchrotron- und Neutronenstrahlung am Pulver einschließlich der D-Lagen geklärt.DPN2: P212121 (Nr. 19), a = 4,6550(2) Å; b = 4,6591(2) Å; c = 7,0560(3) Å, Z = 4, Neutronenbeugung time-of-flight: RBragg (F2o) = 0,0184, 33 Reflexe (d = 1,626 Å - d = 5,278 Å) RBragg (F2o) = 0,0218, 93 Reflexe (d = 1,080 Å - d = 2,623 Å) DPN2 ist aus allseits eckenverknüpften Tetraedern PN4/2 aufgebaut, die ein dreidimensionales Gerüst bilden, wie es unverzerrt im “idealisierten” ß-Cristobalit vorliegt. Die Deuteronen sind geordnet an die Hälfte der N-Atome gebunden.The structure was solved on DPN2 by synchrotron and neutron diffraction data including the D-positions.DPN2: P212121 (Nr. 19), a = 4.6550(2) Å; b = 4.6591(2) Å; c = 7.0560(3) Å, Z = 4, Neutron diffraction time-of-flight: RBragg(F2o) = 0.0184, 33 reflections (d = 1.626 Å - d = 5.278 Å) RBragg(F2o) = 0.0218, 93 reflections (d = 1.080 Å - d = 2.623 Å) DPN2 contains corner-sharing tetrahedra PN4/2. These form a three-dimensional network as it is observed undistorted in “idealized” ß-cristobalite. The deuterons are bonded to one half of the nitrogen atoms in an ordered way.
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  • 45
    ISSN: 0044-2313
    Keywords: Lithiumhydridosiloxysilylamides ; reaction behaviour ; N-silylation ; Si—O bond splitting ; cyclodisilazanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lithium Hydridosiloxysilylamides - Reactions in n-Octane and Tetrahydrofuran in Presence of ChlorotrimethylsilaneThe hydrido-siloxy-silylamino-silanes (Me3SiO)HSiMe(NHSiMe3) 1, (Me3SiO)HSi(NHSiMe3)2 2 and (Me3SiO)2HSi(NHSiMe3) 3 were prepared by coammonolysis of the chlorosiloxysilanes (Me3SiO)HSiMeCl and (Me3SiO)3-nHSiCln (n = 1, 2) with chlorotrimethylsilane. The reaction behaviour of lithiated compounds 1, 2 and 3 has been investigated in n-octane and tetrahydrofuran (THF) in presence of chlorotrimethylsilane.
    Notes: Durch Koammonolyse der Chlorsiloxysilane (Me3SiO)HSiMeCl und (Me3SiO)3-nHSiCln (n = 1, 2) mit Chlortrimethylsilan wurden die Hydrido-siloxy-silylamino-silane (Me3SiO)HSiMe(NHSiMe3) 1, (Me3SiO)HSi(NHSiMe3)2 2 und (Me3SiO)2HSi(NHSiMe3) 3 dargestellt und das Reaktionsverhalten der lithiierten Verbindungen 1, 2 und 3 in n-Octan und Tetrahydrofuran (THF) in Gegenwart von Chlortrimethylsilan untersucht.Sowohl das Monoamid (Me3SiO)HSiMe(NLiSiMe3) als auch das Diamid (Me3SiO)HSi(NLiSiMe3)2 reagieren unter N-Silylierung zu N-Substitutionsprodukten und unter Si—O-Bindungsspaltung und LiOSiMe3-Eliminierung zu Cyclodisilazanen, wobei THF die N-Silylierung, n-Octan die Bildung von Cyclodisilazanen begünstigt. Das Monoamid ergibt in n-Octan (Me3SiO)HSiMe[N(SiMe3)2] 4, [Me(H)Si-NSiMe3]2 5 (Hauptprodukt) und 6, in THF 4 als Hauptprodukt und 5. Aus dem Diamid werden in THF (Me3SiO)HSi[N(SiMe3)2](NHSiMe3) 7, bevorzugt (Me3SiO)HSi[N(SiMe3)2]2 8, [(Me3SiNH)HSi—NSiMe3]2 9 und 10 gebildet, in n-Octan 7, bevorzugt 9 und 10.Hauptprodukt der Reaktion des Amids (Me3SiO)2HSi(NLiSiMe3) in THF und n-Octan ist das N-Silylierungsprodukt (Me3SiO)2HSiN(SiMe3)2 11.Eine Reaktion unter Beteiligung der Si—H-Gruppe wird nur im Falle von (Me3SiO)HSiMe(NLiSiMe3) beobachtet, Produkt dieser Reaktion ist 6.The monoamide (Me3SiO)HSiMe(NLiSiMe3) and the diamide (Me3SiO)HSi(NLiSiMe3)2 react under N-silylation to N-substitution products and under Si—O-bond splitting and LiOSiMe3-elimination to cyclodisilazanes in n-octane as well as in THF. The favour reaction is in THF the N-silylation, in n-octane the formation of cyclodisilazanes. The monoamide gives in n-octane (Me3SiO)HSiMe[N(SiMe3)2] 4, [Me(H)Si-NSiMe3]2 5 (main product) and 6, in THF as main product 4 and 5. The diamide reacts in THF to give (Me3SiO)HSi[N(SiMe3)2](NHSiMe3) 7, mainly (Me3SiO)HSi[N(SiMe3)2]2 8, [(Me3SiNH)HSi—NSiMe3]2 9 and 10, in n-octane 7, mainly 9 and 10.The N-silylation product (Me3SiO)2HSiN(SiMe3)2 11 is the main product of the reaction of (Me3SiO)2HSi(NLiSiMe3) in THF and in n-octane.A reaction with participation of the Si-H group is only observed in the case of (Me3SiO)HSiMe(NLiSiMe3). 6 is the product of this reaction.
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  • 46
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    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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  • 47
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    Zeitschrift für anorganische Chemie 623 (1997), S. 1489-1491 
    ISSN: 0044-2313
    Keywords: 2,9-{N,N′-(2-aminopyridine)}octahydro-closo-decaborate(2-) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [P(C6H5)4][2,9-{N,N′-(2-NH—(C5H4N))}B10H8][N(C4H9)4]2[B10H10] reacts with 2-aminopyridine forming a product mixture from which [2,9-{N,N′-(2-NH—(C5H4N))}B10H8]- can be isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The crystal structure of [P(C6H5)4][2,9-{N,N′-(2-NH—(C5H4N))}B10H8] (triclinic, space group P1, a = 10.1103(9), b = 11.5665(9), c = 14.877(2) Å, α = 102.600(8), β = 107.567(8) und γ = 96.487(7)°, Z = 2) reveals the bonding of 2-NH2-(C5H4N) via both N atoms to vicinal B atoms of the two square planes of the B10 cluster (B2—N1 = 1,541(7) und B9—N2 = 1.505(7) Å) forming a five-membered ring.
    Notes: [N(C4H9)4]2[B10H10] reagiert mit 2-Aminopyridin unter Bildung eines Produktgemisches, aus dem durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose [2,9-{N,N′-(2-NH—(C5H4N))}B10H8]- isoliert werden kann. Die Röntgenstrukturanalyse an [P(C6H5)4][2,9-{N,N′-(2-NH—(C5H4N))}B10H8] (triklin, Raumgruppe P1, a = 10,1103(9), b = 11,5665(9), c = 14,877(2) Å, α = 102,600(8), β = 107,567(8) und γ = 96,487(7)°, Z = 2) beweist, daß 2-NH2-(C5H4N) über beide N-Atome an benachbarte B-Atome der beiden quadratischen Ebenen des B10-Clusters (B2—N1 = 1,541(7) und B9—N2 = 1,505(7) Å) unter Ausbildung eines Fünfringes gebunden ist.
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  • 48
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    Zeitschrift für anorganische Chemie 623 (1997), S. 1483-1488 
    ISSN: 0044-2313
    Keywords: Nonasodium bis(hexahydroxogallate) trihydroxide hexahydrate ; decasodium bis(hexahydroxogallate) tetrahydroxide ; disodium tetrahydroxogallate chloride ; crystal structure ; 71Ga MAS NMR ; 23Na MAS NMR ; DTA, DTG, guinier lenné technique ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Crystalline Sodium HydroxogallatesTwo crystalline sodium hydroxogallates 4,5 Na2O · Ga2O3 · 13,5 H2O (I) and 5 Na2O · Ga2O3 · 8 H2O (II), as well as a crystalline phase of the composition Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) are described.
    Notes: Es werden zwei kristalline Natriumhydroxogallate 4,5 Na2O · Ga2O3 · 13,5 H2O (I) und 5 Na2O · Ga2O3 · 8 H2O (II) sowie eine kristalline Phase der Zusammensetzung Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) beschrieben.(I) kristallisiert aus Natriumgallatlösungen eines breiten Konzentrationsfeldes und hat nach Einkristallröntgenstrukturanalyse [1] eine dreidimensional vernetzte Struktur aus monomeren [Ga(OH)6]3--Anionen, die über NaO6-Koordinationspolyeder untereinander verbunden sind; daneben sind Kristallwasser und weitere Hydroxidionen enthalten.Damit ist (I) als Nonanatrium-bis(hexahydroxogallat)-trihydroxid-hexahydrat (Na9[Ga(OH)6]2(OH)3 · 6 H2O) zu formulieren; Isotypie besteht zu dem entsprechenden Natriumhydroxoaluminat [2, 3]. 5 Na2O · Ga2O3 · 8 H2O II) läßt sich aus (I) in Gegenwart von Natriumhydroxid durch Entwässern über P4O10 bei Raumtemperatur unter Schutzgas (N2) erhalten. Es kristallisiert tetragonal, ist isotyp mit Na10[Al(OH)6]2(OH)4 [4] und dementsprechend als Na10[Ga(OH)6]2(OH)4 zu formulieren. Durch Zusatz von Natriumchlorid zu Natriumgallatlösungen läßt sich Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) isolieren, das ebenfalls tetragonal und isotyp zu Na2[Al(OH)4]Cl [5] ist. Es handelt sich demnach um das Dinatriumtetrahydroxogallatchlorid Na2[Ga(OH)4]Cl. Die Ergebnisse der 71Ga- und 23Na-MASNMR-Messungen an den Verbindungen (I) bis (III) und deren thermisches Verhalten werden diskutiert.(I) crystallizes from sodium gallate solutions in a wide concentration field; from the X-ray single crystal diffraction analysis [1] results a three dimensional network structure, consisting of monomeric [Ga(OH)6]3- anions connected by NaO6 octahedra groups. Furthermore the structure contains water of crystallization and further hydroxide ions. (I) has to be formulated as nonasodium bis(hexahydroxogallate) trihydroxide hexahydrate Na9[Ga(OH)6]2(OH)3 · 6 H2O; it is isotypic with the corresponding sodium hydroxoaluminate [2, 3]. 5 Na2O · Ga2O3 · 8 H2O (II) was obtained from (I) in presence of sodium hydroxide by dehydration over P4O10 in an inert atmosphere (N2) at room temperature. (II) crystallizes tetragonally and is isotypic with Na10[Al(OH)6]2(OH)4 [4]. Accordingly it could be described as a decasodium bis(hexahydroxogallate) tetrahydroxide, Na10[Ga(OH)6]2(OH)4. Na2O · Ga2O3 · 4 H2O · 2 NaCl (III) was obtained by addition of sodium chloride to sodium gallate solutions, (III) crystallizes also tetragonally and is isotypic with (Na2[Al(OH)4]Cl [5]. Correspondingly, it has to be formulated as disodium tetrahydroxogallate chloride Na2[Ga(OH)4]Cl. The results of 71Ga and 23Na MAS NMR investigations of the compounds (I) to (III) and their thermal behaviour are discussed.
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  • 49
    ISSN: 0044-2313
    Keywords: Synthesis ; Crystal structure ; Crown ether ; Lanthanides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3), a Cationic Dimeric in-cavity Complex with Iodide and Triiodide as AnionsSingle crystals of [La2I2(OH)2(dibenzo-18-crown-6)2]I(I3) are obtained from the reaction of LaI3 and dibenzo-18-crown-6 in acetonitrile. The crystal structure monoclinic, C2/m, Z = 4, T = 293 [100] K, a = 2179(3) [2162.3(3)], b = 1070.3(3) [1069.6(1)], c = 1118.2(3) [1110.6(1)] pm, β = 93.1(1) [92.83(1)]°, R1 = 0.0601 [0.0411], wR2 = 0.1449 [0.1014] contains hydroxide-bridged cationic dimers and iodide as well as triiodide as anions.
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  • 50
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    Zeitschrift für anorganische Chemie 623 (1997), S. 1496-1498 
    ISSN: 0044-2313
    Keywords: Guanosine ; Ribofuranoside Ligands ; Antimonate(III) ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyol Metal Complexes. 27. Bis-Diolato Antimonates(III) with Guanosine as the DiolThe complex anions of K3[SbIII(Guo1,2′,3′H-3)2] · 10 H2O (1) and [Co(NH3)6][SbIII(Guo1,2′,3′H-3)2] · 9 H2O (2) are four-coordinate homoleptic bis(diolato)antimonate(III) species. The guanosine trianions act as carbohydrate ligands through their cis-furanoidic ribosyl moiety, thus forming no nucleobase-metal bonds.
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  • 51
    ISSN: 0044-2313
    Keywords: Methylindium Compound ; Heterocubane ; Synthesis ; X-ray Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The X-Ray Structure Determination of tert-Butylimido Methylindane, [CH3In—NC(CH3)3]4The reaction of MeInCl2 with LiN(H)tBu in a 1 : 2 molar ratio forms [MeIn—NtBu]4 in high yield, lithium chloride, and the free amine H2NtBu. The crystal structure of the imidomethylindane with a cubic In4N4 skeleton has been determined.
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  • 52
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    Zeitschrift für anorganische Chemie 623 (1997), S. 1501-1502 
    ISSN: 0044-2313
    Keywords: Cesium yttrium selenide ; Cs3Y7Se12 ; rare-earth compounds ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Crystal Structure of Cs3Y7Se12The oxidation of yttrium metal with selenium in the presence of CsCl (7 d, 700°C, evacuated silicia tubes) results in the formation of pale yellow, lath-shaped single crystals of Cs3Y7Se12. The crystal structure (orthorhombic, Pnnm, Z = 2, a = 1272.8(3), b = 2627.7(5), c = 413.32(8) pm) consists of edge- and vertex-connected [YSe6] octahedra forming a rocksalt-related network [Y7Se12]3-. One-dimensional infinite channels along [001], apt to take up extra cations, provide coordination numbers of 6 and 7 + 1, respectively, for two crystallographically different Cs+.
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  • 53
    ISSN: 0044-2313
    Keywords: Ditetraammine lithium tetraphenyldistannide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH3)4]2[Sn2Ph4]Ruby-red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at -35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1, Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F02 ≥ 4σF02) = 5.13%, wR2 (F02 ≥ 4σF02) = 10.5%, N(F02 ≥ 4σF02) = 779, N(Var.) = 163.The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2- as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].
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  • 54
    ISSN: 0044-2313
    Keywords: Thiazyltrifluoride ; Thiazyldifluoridedimethylamide ; metal complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thiazyltrifluoride NSF3 and Thiazyldifluoridedimethylamide NSF2NMe2: Ligands in Organometallic ChemistryFrom the reaction of [Re(CO)5SO2]+AsF6- (1) and [CpFe(CO)2SO2]+AsF6- (6) with NSF3 (2) and NSF2NMe2 (4) the complexes [Re(CO)5NSF3]+AsF6- (3), [Re(CO)5NSF2NMe2]+AsF6- (5), [CpFe(CO)2NSF3]+AsF6- (7), and [CpFe(CO)2NSF2NMe2]+AsF6- (8) were obtained. The compounds have been characterised by X-ray crystallography, the ligand properties of 2 and 4 are discussed.
    Notes: Durch Umsetzung von [Re(CO)5SO2]+AsF6- (1) und [CpFe(CO)2SO2]+AsF6- (6) mit NSF3 (2) und NSF2NMe2 (4), wurden die Komplexe [Re(CO)5NSF3]+AsF6- (3), [Re(CO)5NSF2NMe2]+AsF6- (5), [CpFe(CO)2NSF3]+AsF6- (7) und [CpFe(CO)2NSF2NMe2]+AsF6- (8) dargestellt und durch Kristallstrukturanalysen charakterisiert. Die Ligandeneigenschaften von 2 und 4 werden diskutiert.
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  • 55
    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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  • 56
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    Zeitschrift für anorganische Chemie 623 (1997), S. 1529-1534 
    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.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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    ISSN: 0044-2313
    Keywords: Oxidative addition reactions ; ionic binuclear tetrakis(triphenylphosphine)-(μ-fluoro)-(μ-peroxo)-platinum(II)-fluorosulphonate and -methylsulphonate complexes ; dynamic behaviour ; O,O-sulfito-manganese(II) tricarbonyl complexes ; bis-η5-cyclopentadienyl- and μ-disulfito-dimetalhexa- and -decacarbonyl complexes (metal = Mn, Mo, W) ; Chemistry ;