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  • 1
    Electronic Resource
    Electronic Resource
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 52 (1996), S. 453-455 
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The structure of the title compound [N,N'-methylenedipyridinium 1-iodononahydro-closo-decaborate(2-), C11H12N2+2.B10H9I2−] has been determinated by single-crystal X-ray diffraction at room temperature. This is the first halogeno derivative of closo-[B10H10]2− with the substituent in the apical position. The square pyramid with the capping ipso-B atom is slightly compressed. The B—I distance of 2.209 (6) Å in [1-IB10H9]2− is significantly shorter than the distance of 2.230 (2) Å in the [2-IB10H9]2− isomer.
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  • 2
    ISSN: 0044-2313
    Keywords: Halogeno-nonahydro-closo-decaborates(2-) ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of Dipyridiniomethane Monohalogenohydro-closo-Decaborates(2-), [(C5H5N)2CH2][2-XB10H9]; X = Cl, Br, I[B10H10]2- reacts with chlorine, bromine and iodine or with N-halogenosuccinimide, yielding the monohalogenodecaborates [2-XB10H9]2- (X = Cl, Br, I), which are separated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose from the starting compound and higher halogenated products. The X-ray structure determinations of the isotypic chloro and bromo compounds [(C5H5N)2CH2][2-XB10H9] (monoclinic, space group C2/c, Z = 8; for X = Cl: a = 33.174(5), b = 7.2809(4), c = 16.2232(7) Å, β = 113.307(7)°; for X = Br: a = 33.525(11), b = 7.281(2), c = 16.297(4) Å, β = 113.62(2)°) and of the iodo compound [(C5H5N)2CH2][2-IB10H9] (monoclinic, space group P21, Z = 2, a = 7.143(3), b = 13.568(4), c = 9.479(7) Å, β = 97.57(5)°) show columns of substituted boron clusters [2-XB10H9]2-, X = Cl, Br, I and bent dications [(C5H5N)2CH2]2+ along the shortest axis wich are assembled to alternating layers in the crystal lattice.
    Notes: [B10H10]2- reagiert mit Chlor, Brom und Iod bzw. mit N-Halogensuccinimid zu den entsprechenden Monohalogenodecaboraten [2-XB10H9]2- (X = Cl, Br, I). Die Verbindungen werden durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose von der Ausgangssubstanz und höher halogenierten Produkten getrennt. Die Röntgenstrukturanalysen der isotypen Chloro- und Bromoverbindungen [(C5H5N)2CH2][2-XB10H9] (monoklin, Raumgruppe C2/c, Z = 8; für X = Cl: a = 33,174(5), b = 7,2809(4), c = 16,2232(7) Å, β = 113,307(7)°; für X = Br: a = 33,525(11), b = 7,281(2), c = 16,297(4) Å, β = 113,62(2)°) und der Iodoverbindung [(C5H5N)2CH2][2-IB10H9] (monoklin, Raumgruppe P21, Z = 2, a = 7,143(3), b = 13,568(4), c = 9,479(7) Å, β = 97,57(5)°) zeigen im Kristallgitter Stränge der substituierten Clusteranionen [2-XB10H9]2-, X = Cl, Br, I und der Dikationen [(C5H5N)CH2]2+ in Richtung der kürzesten Achse, die in alternierenden Schichten angeordnet sind.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    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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  • 4
    ISSN: 0044-2313
    Keywords: Monothiocyanato-nonahydro-closo-decaborate(2-) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tetraphenylphosphonium Monothiocyanatohydro-closo-Decaborate, [P(C6H5)4]2[2-(SCN)B10H9] · CH3CNThe X-ray structure determination of [P(C6H5)4]2[2-(SCN)B10H9] · CH3CN (monoclinic, space group P21/n, a = 10.6040(10), b = 13.8880(9), c = 33.888(3) Å, β = 94.095(8)°, Z = 4) reveals the S coordination of the SCN substituent with a B—S distance of 1.913(6) Å and a B—S—C angle of 105.3(3)°. The SCN group is nearly linear (178.2(7)°).
    Notes: Die Röntgenstrukturanalyse an [P(C6H5)4]22-(SCN)B10H9· CH3CN (monoklin, Raumgruppe P21/n, a = 10,6040(10), b = 13,8880(9), c = 33,888(3) Å, β = 94,095(8)°, Z = 4) beweist die Bindung des Thiocyanatsubstituenten über das S-Atom mit einem B—S-Abstand von 1,913(6) Å unter dem B—S—C-Bindungswinkel von 105,3(3)°. Die SCN-Gruppe ist mit 178,2(7)° annähernd linear.
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  • 5
    ISSN: 0044-2313
    Keywords: 1-Nitro-nonahydro-closo-decaborate(2-) ; Crystal Structure ; 11B NMR Spectrum ; Vibrational Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, 11B NMR, Vibrational Spectra, and Crystal Structure of [(C5H5N)2CH2][1-(O2N)B10H9]By reaction of [B10H10]2- in aqueous acetonitrile with a saturated solution of NO2 in dichloromethane [1-(O2N) · B10H9]2- and [B10H9(NO)B10H9]3- are formed which can be separated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose from the starting compound. The X-ray structure determination of [(C5H5N)2CH2][1-(O2N)B10H9] (triclinic, space group P1, a = 7.1530(9), b = 8.3753(8), c = 15.198(2) Å, α = 96.00(1), β = 95.48(1), γ = 95.60(1)°, Z = 2) reveals the coordination of the NO2 group via N with a B1—N distance of 1.535(5) Å and an O2—N—O1 angle of 119.3(3)°. The 11B NMR spectrum exhibits the characteristic feature (1 : 1 : 4 : 4) of an apical monosubstituted B10 cluster with a strong downfield shift of the ipso-B atom at +13.4 ppm. The IR and Raman spectra show strong NO stretching vibrations at 1381 und 1420 cm-1.
    Notes: [B10H10]2- reagiert in wäßrigem Acetonitril mit einer gesättigten Lösung von NO2 in Dichlormethan zu [1-(O2N)B10H9]2- und [B10H9(NO)B10H9]3-, die durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose von der Ausgangssubstanz getrennt werden. Die Röntgenstrukturanalyse an [(C5H5N)2CH2][1-(O2N)B10H9] (triklin, Raumgruppe P1, a = 7,1530(9), b = 8,3753(8), c = 15,198(2) Å, α = 96,00(1), β = 95,48(1), γ = 95,60(1)°, Z = 2) beweist die Bindung der NO2-Gruppe über das N-Atom mit einem B1—N-Abstand von 1,535(5) Å unter dem O2—N—O1-Bindungswinkel von 119,3(3)°. Im 11B-NMR-Spektrum beobachtet man das charakteristische Signalmuster (1 : 1 : 4 : 4) eines in 1-Position substituierten B10-Clusters mit starkem Tieffeldshift des ipso-B-Kerns bei +13,4 ppm. Im IR- und Raman-Spektrum treten intensive NO-Valenzschwingungen bei 1381 und 1420 cm-1 auf.
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  • 6
    ISSN: 0044-2313
    Keywords: 1-Ammine-nonahydro-closo-decaborate(1-) ; Ammine-undecahydro-closo-dodecaborate(1-) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structures of [P(C6H5)4][1-(NH3)B10H9] and Cs[(NH3)B12H11] · 2CH3OHThe reduction of [1-(NO2)B10H9]2- with aluminum in alkaline solution yields [1-(NH3)B10H9]- and by treatment of [B12H12]2- with hydroxylamine-O-sulfonic acid [(NH3)B12H11]- is formed. The crystal structures of [P(C6H5)4][1-(NH3)B10H9] (triclinic, space group P1, a = 7.491(2), b = 13.341(2), c = 14.235(1) Å, α = 68.127(9), β = 81.85(2), γ = 86.860(3)°, Z = 2) and Cs[(NH3)B12H11] · 2CH3OH (monoclinic, space group P21/n, a = 14.570(2), b = 7.796(1), c = 15.076(2) Å, β = 111.801(8)°, Z = 4) reveal for both compounds the bonding of an ammine substituent to the cluster anion.
    Notes: Die Reduktion von [1-(O2N)B10H9]2- mit Aluminium in alkalischer Lösung ergibt [1-(NH3)B10H9]-, bei der Umsetzung von [B12H12]2- mit Hydroxylamin-O-sulfonsäure bildet sich [(NH3)B12H11]-. Die Röntgenstrukturanalysen an [P(C6H5)4][1-(NH3)B10H9] (triklin, Raumgruppe P1, a = 7,491(2), b = 13,341(2), c = 14,235(1) Å, α = 68,127(9), β = 81,85(2), γ = 86,860(3)°, Z = 2) und Cs[(NH3)B12H11] · 2CH3OH (monoklin, Raumgruppe P21/n, a = 14,570(2), b = 7,796(1), c = 15,076(2) Å, β = 111,801(8)°, Z = 4) beweisen, daß in beiden Fällen ein Ammin-Substituent am Clusteranion vorliegt.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 347-350 
    ISSN: 0044-2313
    Keywords: 1-Monothiocyanato-nonahydro-closo-decaborate(2-) ; 1,10-Dithiocyanato-octahydro-closo-decaborate(2-) ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structures of (PPh4)2[1-(SCN)B10H9] and (AsPh4)2[1,10-(SCN)2B10H8]By reaction of [B10H10]2- with (SCN)2 in dichloromethane mixtures of thiocyanato-hydro-closo-decaborates are formed. The crystal structures of (PPh4)2[1-(SCN)B10H9] (monoclinic, space group P 21/a, a = 20.245(2), b = 10.434(9), c = 22.235(3) Å, β = 90.951(10)°, Z = 4) and (AsPh4)2[1,10-(SCN)2B10H8] (triclinic, space group PP1, α = 10.598(2), b = 13.057(3), c = 19.902(3) Å, α = 104.37(2), β = 91.725(11), γ = 110.35(2)°, Z = 2) reveal for both compounds the bonding of the SCN substituents via the S atom.
    Notes: Bei der Umsetzung von [B10H10]2- mit (SCN)2 in Dichlormethan entstehen Gemische aus Thiocya nato-hydro-closo-decaboraten. Die Röntgenstrukturanalyse an (PPh4)2[l-(SCN)B10H9] (monoklin, Raumgruppe P21/a, a = 20,245(2), b = 10,434(9), c = 22,235(3) Å, β = 90,951(10)°, Z = 4) und (AsPh4)2[1,10-(SCN)2B10H8] (triklin, Raumgruppe P1, a = 10,598(2), b = 13.057(3), c = 19,902(3) Å, α = 104,37(2), β =91,725(11), γ =110,35(2)°, Z = 2) beweist in beiden Fällen die Bindung der SCN-Substituenten über das S-Atom.
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  • 8
    ISSN: 0044-2313
    Keywords: 1,10-Dinitro-octahydro-closo-decaborate(2-) ; Crystal Structure ; 11B NMR Spectrum ; Vibrational Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, 11B NMR, Vibrational Spectra and Crystal Structure of [P(C6H5)4]2 [1,10-(O2N)2B10H8]By reaction of [N(C4H9)4]2[B10H10] in aqueous acetonitrile with NO2 a reaction mixture is formed from which [1,10-(O2N)2B10H8]2- has been isolated by ion exchange chromatography on diethylaminoethyl(DEAE) cellulose. The X-ray structure determination of [P(C6H5)4]2 [1,10-(O2N)2B10H8] (triclinic, space group P1, a = 10.831(3), b = 13.059(3), c = 18.496(5) Å, α = 82.13(2), β = 75.87(2), γ = 71.08(2)°, Z = 2) reveals the coordination of both nitro groups via N in the apical positions of the B10 cluster with B1-N1 = 1.526(3) and B10-N2 = 1.537(3) Å and ONO angles of 119.3(2) and 120.1(2)°. The 11B NMR spectrum exhibits the characteristic feature (2:8) of a in 1,10 position disubstituted B10 cluster with a strong downfield shift of the ipso-B atoms at + 17.3 ppm. The IR and Raman spectra show strong NO stretching vibrations at 1384 und 1425 cm-1.
    Notes: Beim Einleiten von NO2 in eine wäßrige Acetonitrillösung von [N(C4H9)4]2 [B10H10] entsteht ein Produktgemisch, aus dem [1,10-(O2N)2B10H8]2- durch Ionenaustauschchromatographie an Diethylaminoethyl(DEAE)-Cellulose isoliert worden ist. Die Röntgenstrukturanalyse an [P(C6H5)4]2 [1,10-(O2N)2B10H8] (triklin, Raumgruppe P1, a = 10,831(3), b = 13,059(3), c = 18,496(5) Å, α = 82,13(2), β = 75,87(2), γ = 71,08(2)°, Z = 2) beweist die Bindung der beiden Nitro-Gruppen über die N-Atome in apikaler Position des B10-Clusters mit den Abständen von B1-N1 = 1,526(3) und B10-N2 = 1,537(3) Å und den ONO-Winkeln 119,3(2) und 120.1(2)°. Im 11B-NMR-Spektrum beobachtet man das charakteristische Signalmuster (2:8) eines in 1,10-Position disubstituierten B10-Clusters mit starkem Tieffeldshift der ipso-B-Kerne bei + 17,3 ppm. Im IR- und Raman-Spektrum treten intensive NO-Valenzschwingungen bei 1384 und 1425 cm-1 auf.
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