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  • 1
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 2
  • 3
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 4
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 5
    ISSN: 0044-2313
    Keywords: Tetraarsenidometallates(V) ; Heptaalkalitetraarsenidniobates(V) ; Heptaalkalitetraarsenidotantalates(V) ; stuffed shear variant of Na6□ZnO4 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Properties of the Tetraarsenidometallates(V) M7[TAs4] (M = K, Rb; T = Nb, Ta)The tetraarsenidometallates(V) M7[TAs4] (M = K, Rb; T = Nb, Ta) have been prepared from RbAs, KAs, Rb3As, K3As, and Nb or Ta in sealed Nb(Ta) ampoules at T = 1100 K. They crystallize in a new structure type oP24 (Pmn21, no. 31); K7[NbAs4]: a = 1019.2(2) pm, b = 916.2(2) pm, c = 830.6(1) pm; K7[TaAs4]: a = 1017.3(2) pm, b = 915.5(2) pm, c = 830.5(2) pm; Rb7[NbAs4]: a = 1059.2(4) pm, b = 952.8(4) pm, c = 860.4(4) pm; Z = 2 formula units per unit cell). The compounds form dark red crystals and they are sensitive against air and moisture. They are semiconductors with Eg = 1.80 eV. The thermal decomposition in dynamical vacuum gives evidence for the existance of K4TAs3 and K2TAs2 (T = Nb, Ta). Main structural units are polar oriented tetrahedra [TAs4] with d(T - As) = 252.2(1) pm; 251.3(1) pm; 253.0(4) pm, respectively. The As atoms are trigonal prismatically coordinated by M and T atoms. These trigonal prisms form anionic and cationic layers ∞2[M4As2]2- and ∞2[M3TAs2]2+ alternating along the b axis. The structure is comparable with that of Co2P and can be described as a stuffed shear variant of the Na6□ZnO4 type of structure.
    Notes: Die Tetraarsenidometallate(V) M7[TAs4] (M = K, Rb; T = Nb, Ta) wurden aus RbAs, KAs, Rb3As, K3As und elementarem Nb bzw. Ta in geschlossenen Nb(Ta)-Ampullen bei 1100 K dargestellt. Sie kristallisieren in einem neuen Strukturtyp oP24 (Pmn21, Nr. 31); K7[NbAs4]: a = 1019.2(2) pm, b = 916.2(2) pm, c = 830.6(1) pm; K7[TaAs4]: a = 1017.3(2) pm, b = 915.5(2) pm, c = 830.5(2) pm; Rb7[NbAs4]: a = 1059.2(4) pm, b = 952.8(4) pm, c = 860.4(4) pm; Z = 2 Formeleinheiten). Die luft- und hydrolyseempfindlichen Verbindungen bilden dunkelrote, quaderförmige Kristalle. Sie sind Halbleiter mit Eg = 1.80 eV. Der thermische Abbau im dynamischen Vakuum liefert Hinweise auf die Existenz von K4TAs3 und K2TAs2 (T = Nb, Ta). Wesentliche Baueinheiten sind polar ausgerichtete [TAs4]-Tetraeder mit d (T - As) = 252.2(1) pm, 251.3(1) pm bzw. 253.0(4) pm. Die As-Atome sind trigonal-prismatisch von M- und T-Atomen umgeben. Diese trigonalen Prismen bilden entlang der b-Achse abwechselnd anionische und kationische Schichten, ∞2[M4As2]2- bzw. ∞2[M3TAs2]2+. Die Strukturen sind mit der von Co2P vergleichbar und können als aufgefüllte Schervarianten der Na6□ZnO4-Struktur aufgefaßt werden.
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  • 6
    ISSN: 0044-2313
    Keywords: Tetrapnictidotitanate(IV) ; centered heterocubanes ; hierarchical derivative of Cr3Si and KGe ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetrapnictidotitanates(IV) M4TiX4 (M = Sr, Ba; X = P, As), hierarchical Derivatives of the KGe Structure K4□Ge4The four new tetrapnictidotitanates(IV) Sr4TiP4, Sr4TiAs4, Ba4TiP4 and Ba4TiAs4 are synthesized from the binary pnictides MX (M = Sr, Ba and X = P, As) and elementary titanium in tantalum ampoules. The compounds are isotypic and isoelectronic with Ba4SiAs4 (space group P43n (no. 218); cP72; Z = 8; Sr4TiP4: a = 1259.0(1) pm; Sr4TiAs4: a = 1288.3(4) pm; Ba4TiP4: a = 1316.6(2) pm; Ba4TiAs4: a = 1346.9(2) pm). The transition metal compounds form cubic, metallic reflecting crystals (Sr4TiP4 (green); Sr4TiAs4 (silver coloured); Ba4TiP4 (silver coloured); Ba4TiAs4 (violet). They are semiconducting and very sensitive against air and moisture. The structure is a hierarchical derivative of Cr3Si (A15) and KGe type: Cr6Si2 ≙ (□Ge4K4)6(□Ge4K4)2 ≙ (TiX4M4)6(TiX4M4)2, where Ti occupies the positions of the Cr3Si structure, and the alkaline-earth metal and pnicogen atoms occupy the positions of the KGe structure. Therefore, Ti is surrounded by four X and four more distant M atoms forming a heterocubane. The mean bond lengths are: d(Ti—P) = 238.0(5) pm; 307 ≤ d(Sr—P) ≤ 333 pm; d(Ti—As) = 245.9(4); 313 ≤ d(Sr—As) ≤ 341 pm; d(Ti—P) = 240.5(5); 324 ≤ d(Ba—P) ≤ 348 pm; d(Ti—As) = 248.3(3) pm; 331 ≤ d(Ba—As) ≤ 355 pm.
    Notes: Die vier neuen Tetrapnictidotitanate(IV) Sr4TiP4, Sr4TiAs4, Ba4TiP4 und Ba4TiAs4 wurden aus den binären Komponenten MX (M = Sr, Ba und X = P, As) und elementarem Titan in Tantalampullen dargestellt. Alle Verbindungen sind isotyp und isoelektronisch zu Ba4SiAs4 (Raumgruppe P43n (Nr. 218), cP72, Z = 8; Sr4TiP4: a = 1259.0(1) pm; Sr4TiAs4: a = 1288.3(4) pm; Ba4TiP4: a = 1316.6(2) pm; Ba4TiAs4: a = 1346.9(2) pm). Die Übergangsmetallverbindungen bilden würfelförmige, metallisch reflektierende Kristalle (Sr4TiP4 (grün), Sr4TiAs4 (silberfarben) Ba4TiP4 (silberfarben), Ba4TiAs4 (violett). Sie sind halbleitend und sehr empfindlich gegenüber Luft und Feuchtigkeit. Die Struktur ist eine hierarchische Variante vom Cr3Si- (A15) und KGe-Typ: Cr6Si2 ≙ (□Ge4K4)6(□Ge4K4)2 ≙ (TiX4M4)6(TiX4M4)2, in der die Ti-Atome die Positionen der Cr3Si-Struktur, die Erdalkalimetall- und Pnicogenatome die Positionen der KGe-Struktur besetzen. Ti ist deshalb von vier X-Atomen und von vier weiter entfernten M-Atomen in Form eines Heterokubans umgeben. Die mittleren Bindungslängen sind: d(Ti—P) = 238.0(5) pm, 307 ≤ d(Sr—P) ≤ 333 pm; d(T—As) = 245.9(4), 313 ≤ d(Sr—As) ≤ 341 pm; d(Ti—P) = 240.5(5), 324 ≤ d(Ba—P) ≤ 348 pm; d(Ti—As) = 248.3(3) pm, 331 ≤ d(Ba—As) ≤ 355 pm.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 442 (1978), S. 91-94 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Dodecamethyl-hexasila-tetraphospha-adamantane (Sime2)6P4Dodecamethyl-hexasila-tetraphospha-adamantane (Sime2)6P4 crystallizes in the cubic space group I 43m with a = 1081.7 pm and Z = 2 formula units. The bond lengths are P—Si = 224.9 pm, C—Si = 186.4 pm and C—H = 87 pm. The bond angles at the P-atoms are 104.4° and at the Si-atoms 118.8°. - The structure of the isotypic compound (Geme2)6P4 was refined.
    Notes: Dodekanmethyl-hexasila-tetraphospha-adamantan (Sime2)6P4 kristallisiert kubisch in der Raumgruppe I 43m mit a = 1081,7 pm und Z = 2 Formeleinheiten. Die Bindungslängen sind P—Si = 224,9 pm, C—Si = 186,4 pm und C—H = 87 pm. Die Bindungswinkel betragen an den P-Atomen 104,4° und an Si-Atomen 118,8°. - Die Struktur der isotypen Verbindung (Geme2)6P4 wurde verfeinert.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 442 (1978), S. 107-111 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure of 2,2,5,5,7,7-Hexamethyl-3,6-di-t-butyl-1,3,4,6-tetraphospha-2,5,7-trisila-norbornane (me2Si)3P4(Cme3)22,2,5,5,7,7-Hexamethyl-3,6-di-t-butyl-1,3,4,6-tetraphospha-2,5,7-trisila-norbornane(me2Si)3P4(Cme3)2 crystallizes monoclinic in the space group C2/c with a = 1593.2 pm, b = 1177.5 pm, c = 1373.3 pm, ß = 111.39° and Z = 4 formula units. In the central norbornane framework the bond lengths are P—P = 221.4 pm, P—Si = 225.9 pm, respectively. The bond lengths to the substituents are P—C = 189.1 pm and Si—C = 188.0 pm. Configuration and conformation are discussed in detail.
    Notes: 2,2,5,5,7,7-Hexamethyl-3,6-di-t-butyl-1,3,4,6-tetraphospha-2,5,7-trisilanorbornan (me2Si)3P4(Cme3)2 kristallisiert monoklin in der Raumgruppe C2/c mit a = 1593,2 pm, b = 1177,5 pm, c = 1373,3 pm, ß = 111,39° und Z = 4 Formeleinheiten. Im zentralen Norbonan-Gerüst sind die Abstände P—P = 221,4 pm und P—Si = 225,9 pm bzw. 229,1 pm. Zu den Substituenten sind die Abstände P—C = 189,1 pm und Si—C = 188,0 pm. Konfiguration und Konformation werden eingehend diskutiert.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 465 (1980), S. 72-82 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structures of the Heptahetero-Nortricyclene-chromiumcarbonyl Complexes P4(Sime2)3Cr(CO)5 and [P4(Sime2)3Cr(CO)4]2Hexamethyl-trisila-tetraphospha-norticyclene-chromium-pentacarbonyl P4(Sime2)3Cr(CO)5 1 and Bis-hexamethyl-trisila-tetraphospha-nortricyclene-chromiumtetracarbonyl [P4(Sime2)3Cr(CO)4]2 2 are nortricyclene complexes with P atoms of the P3 ring acting as donor atoms. The crystal and molecular structures were determined by single crystals (1; space group P1 (No.2); a = 992.4 pm, b = 1301.7 pm, c = 895.7 pm, α = 91.15°, β = 105.650, γ = 98.74°, Z = 2; MoKα radiation, 3978 hkl, R = 0.032; 2; space group Pbca (No. 61); a = q715.6 pm, b = 4003.4 pm, c = 1254,8 pm, Z = 8; MoKα radiation, 3745 hkl, R = 0.070). The bond distances P —Cr are 240.3 pm and 238.1 pm, respectively. The bonding of the chromiumcarbonylgroups to the P3 ring leads only to small changes of the bond distances (1-2 pm) in the nortricyclene system. The bond angles around the donor atom change cooperatively to a more tetrahedral configuration at the donor atom. These changes are discussed in detail.
    Notes: Hexamethyl-trisila-tetraphospha-Nortricyclen-chrompentacarbonyl P4(Sime2)3Cr(CO)5 1 und Bis-hexamethyl-trisila-tetraphospha-Nortricyclen-chromtetracarbonyl [P4(Sime2)3Cr(CO)4]2 2 sind Nortricyclen-Komplexe mit Phosphoratomen des 3-Rings als Donatoren. Die Kristall- und Molekülstrukturen wurden an Einkristallen bestimmt (1; Raumgruppe P1 (Nr. 2); a = 992.4 pm; b = 1301,7 pm; c = 895,7 pm; α = 91,15°; β = 105,65°; γ = 98,74°; Z = 2; MoKαStrahlung; 3978 hkl; R = 0,032. 2; Raumgruppe Pbca (Nr.61); a = 1715,6 pm; b = 4003,4 pm; c = 1254,8 pm; Z = 8; MoKαStrahlung; 3745 hkl; R = 0,070). Die Abstände P—Cr betragen 240,3 pm bzw. 238,1 pm. Die Bindung von Chromcarbonylgruppen an den P3-Ring führt zu geringfügigen Veränderungen bei den Bindungsabständen (1-2 pm) des Nortricyclensystems. Die Bindungswinkel im weiteren Bereich der Donoratome ändern sich jedoch deutlich kooperativ im sinne der Ausbildung einer Tetraederkonfiguration am Donor. Die Veränderungen werden eingehend diskutiert.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 552 (1987), S. 69-80 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry and Structural Chemistry of Phosphides and Ployphosphides. 44. Tricesium Heptaphosphide Cs3P7: Preparation, Structure, and PropertiesTricesium heptaphosphide is prepared from the elements by a quantitative reaction at 1200 K in Nb ampoules. Slow cooling yield the bright yellow α-Cs3P7, quenching the yellow orange coloured β-Cs3P7. The crystalline α-Cs3P7 transforms at 552 K in a first order phase transition to the plastically crystalline β-Cs3P7. Both modifications are sensitive against moisture and oxygen and are completely soluble in ethylendiamine yielding a pale yellow solution. At room temperature the 31P nmr spectra of such solutions show only one singulett, which corresponds to the valence tautomerism of the P73- anion. α-Cs3P7 crystallizes in a new structure type (P41, a = 904.6(1) pm; c = 1671.4(4) pm; Z = 4). The structure is formed by heptaphospha-nortricyclene anions P73- and Cs+ cations. The cs atoms connect the anions forming a three-dimensional arrangement (d̄(Cs—P) = 374 pm), not allowing the fragmentation into discrete Cs3P7 units. The P—P distances differ by their function in the nortricyclene anion. Each P7 group is surrounded by 12 Cs atms. β-Cs3P7 crystallizes in the Li3Bi type of structure (Fm3M; a(573 K) = 1130.5(1)pm; Z = 4). The P atoms of the P73- anions surround the Bi positions with an orienational disorder. The orientation has been investigated with a mixed crystal Ca3(P7)2/3(P11)1/2 (Fm3m; a (298 K) = 1149.5(9) pm; Z = 4).
    Notes: Tricäsiumheptaphosphid wird durch quantitativen Umsatz der Elemente bei 1200 K in Niob-Ampullen erhalten. Beim langsamen Abkühlen erhält man leuchtend gelbes α-Cs3P7, bei schnellem Abkühlen das gelborangefarbene β-Cs3P7. α-Cs3P7 wandelt sich bei 552 K in einem strukturellen Phasenübergang reversibel in plastisch-kristallines β-Cs3P7 um. Beide Modifikationen sind sauerstoff-und feuchtigkeitsempfindlich und lösen sich rückstandsfrei in Ethylendiamin zu einer blaßgelben Lösung. Das 31P NMR-Spektrum dieser Lösungen zeigt bei 298 K das Singulett (δ = 115,5) der valenztautomeren Formen des P73--Anions. α-Cs3P7 kristallisiert in einem neuen Strukturtyp (P41; a = 904,6(1) pm; c = 1671,4(4)pm; Z = 4). Die Struktur wird aus Hepta-phosphanortricyclen-Anionen P73- und Cs+-Kationen aufgebaut. Die Cs-Atome verknüpfen die Anionen zu einer dreidimensionalen struktur (d̄(Cs-P) = 374pm), die nicht in moleklare Einheiten Cs3P7 separiebar ist. Die P—P-Abstände im P7-Gerüst ändern sich in typischer Weise mit der Funktion der Bindungen. Jede P7-Gruppe ist von 12 Cs-Atomen umgeben. β-Cs3P7 kristallisiert im Li3Bi-Typ (Fm3m; a (573 K) = 1130,5(1) pm; Z = 4). Die P-Atome der P73--Anionen umgeben die Bi-Positionen mit einer Orientierungsfehlordnung. Die Orientierung wurde am Beispiel eines MischkristallesCs3(P7)2/3(P11)1/3 untersucht (Fm3m; a(298 K) = 1149,5(9) pm; Z = 4).
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