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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 127 (1996), S. 1215-1220 
    ISSN: 1434-4475
    Keywords: Coordination of As(III) ; Structure ; Stereoisomeres
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Arsenictris(trifluoroacetate) (1) crystallizes monoclinic in the space group Cc witha=1229.3,b=1697.9,c=1243.5 pm, β=110.01°, andZ=8. The trifluoroacetic acid ions acts as chelating ligands. Additionally they are bridging crystallographic independent molecules. As has a coordination number of 3+3(+2). The unit cell contains two sets of chirameres.
    Notes: Zusammenfassung Arsen-tris(trifluoracetat) (1) kristallisiert monoklin in der Raumgruppe Cc mita=1229.3,b=1697.9,c=1243.5 pm, β=110.01° undZ=8. Die Trifluoracetatanionen fungieren gegenüber As als zweizähnige Liganden und verknüpfen die beiden kristallographisch unabhängigen Moleküle zusätzlich intermolekular. As erreicht dadurch gegenüber O die Koordinationszahl 3+3(+2). Die Elementarzelle enthält zwei Sätze von chirameren Molekülen.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 127 (1996), S. 461-468 
    ISSN: 1434-4475
    Keywords: Coordination of As(III) and Sb(III) ; Structure ; Enantiomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Arsen-tris(2,2-dimethylpropionate) (1) crystallizes monoclinic in the space group P21/n witha=926.2,b=2158.6,c=983.7 pm, β=94.92°, andZ=4. As has a coordination number of 3+3. Antimony tripropionate (2) crystallizes monoclinic in the space group P21/c witha=930.2,b=863.0,c=1575.2 pm, β=90.27, andZ=4. The molecules are bridged to chains; therefore, Sb reaches the coordination number 3+3 (+3).
    Notes: Zusammenfassung Arsen-tris(2,2-dimethylpropionat) (1) kristallisiert monoklin in der Raumgruppe P21/n mita=926.2,b=2158.6,c=983.7 pm, β=94.92° undZ=4. As hat gegenüber O die Koordinationszahl 3+3. Antimontripropionat (2) kristallisiert monoklin in der Raumgruppe P21/c mita=930.2,b=863.0,c=1575.2 pm, β=90.27 undZ=4. Die Moleküle sind intermolekular zu Ketten verknüpft, wodurch Sb die Koordinationszahl 3+3 (+3) erreicht.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1038-1046 
    ISSN: 0044-2313
    Keywords: Binuclear antimony(V) complexes ; structure ; dynamics ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: d, h-μ-Benzylalkoxophosphonato-e-μ-alkoxo-f-μ-oxo-bis[trichloroantimony(V)] CompoundsThe binuclear antimony(V) complexes Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 - 6 with R1 = R2 = CH3, C2H5 and R3 = C6H5CH2, (CH3)3C6H2CH2 in solution slowly exchanges the R2 groups between the oxygen atoms of the Sb2O2 ring. The SbOPOSb ringsystem makes rapid pseudorotation. The isomeres are detected by nmr spectroscopy. 1 (R1 = R2 = CH3) crystallizes in the orthorhombic space group Pnma with a = 1247.0, b = 1324.1, c = 1207.9 pm and Z = 4. 2 (R1 = CH3, R2 = C2H5) and 5 (R1 = R2 = CH3, R3 = (CH3)3 · C6H2CH2) crystallizes triclinic in the space group P-1 with a = 984.1, b = 1026.7, c = 1079.9 pm, α = 87.93, β = 75.70, γ = 87.62° and Z = 2 and a = 1164.6, b = 1296.9, c = 1712.9 pm, α = 109.9, β = 96.3, γ = 100.2° and Z = 4 resp., with two crystallographically independent molecules in the asymmetric unit.
    Notes: Die zweikernigen Antimon(V)-Komplexe Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 bis 6 mit R1 = R2 = CH3, C2H5 und R3 = C6H5CH2, (CH3)3C6H2CH2 tauschen bei RT in Lösung langsam die R2-Gruppen aus. Daneben erfolgt rasches Umklappen des SbOPOSb-quasi-Fünfringes. Die Isomerenbildung wird NMR-spektroskopisch nachgewiesen. 1 (R1 = R2 = CH3) kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 1247,0, b = 1324,1, c = 1207,9 pm und Z = 4. 2 (R1 = CH3, R2 = C2H5) und 5 (R1 = R2 = CH3, R3 = (CH3)3C6H2CH2) kristallisieren triklin in der Raumgruppe P-1 mit a = 984,1, b = 1026,7, c = 1079,9 pm, α = 87,93, β = 75,70, γ = 87,62° und Z = 2 bzw. a = 1164,6, b = 1296,9, c = 1712,9 pm, α = 109,9, β = 96,3, γ = 100,2° und Z = 4 mit zwei kristallographisch unabhängigen Molekülen in der asymmetrischen Einheit.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1633-1638 
    ISSN: 0044-2313
    Keywords: (CH3)2S derivatives ; Structure ; Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (CH3)2SBr2 - Reactions and Structures(CH3)2SBr2 (1) is a donor acceptor complex (8-S-3 + 10-Br-2) which reacts with (CH3)2S(=O)NSi(CH3)3 to yield [(CH3)2S(O)=N—S(CH3)2]+Br- (2). With SbBr3 (CH3)2SBr+SbBr4- (3) can be isolated. 1 crystallizes monoclinic in the space group P21/c with a = 733.8, b = 734.2, c = 1132.7 pm, β = 92.8° and Z = 4. 2 crystallizes in the orthorhombic space group Pnma with a = 967.2, b = 793.3, c = 1168.3 pm and Z = 4. The SBr and BrBr force constants of 1 are compared with those of S2Br2, 3 and Br2 resp. The nmr and mass spectra of 1 and 2 are communicated.
    Notes: (CH3)2SBr2 (1) ist ein (8-S-3 + 10-Br-2) Donor-Akzeptor-Komplex(8-S-3 + 10-Br-2) bedeutet: acht Valenzelektronen am S-Atom, das von drei Bindungspartnern umgeben ist, und zehn Valenzelektronen am Br-Atom, das zwei Bindungspartner hat; s.: S. W. Perkins, J. C. Martin, A. J. Arduengeo III, W. Lau, A. Alegria, J. K. Kochi, J. Am. Chem. Soc. 1980, 102, 7753. und reagiert mit (CH3)2S(=O)NSi(CH3)3 zu [(CH3)2S(O)=N—S(CH3)2]+Br- (2), mit SbBr3 zu (CH3)2SBr+SbBr4- (3). 1 kristallisiert monoklin (P21/c) mit a = 733,8, b = 734,2, c = 1132,7 pm, β = 92,8° und Z = 4. 2 kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 967,2, b = 793,3, c = 1168,3 pm und Z = 4. Die SBr- und BrBr-Kraftkonstanten von 1 werden mit denen von S2Br2 und 3 bzw. Br2 verglichen. Die NMR- und Massenspektren von 1 und 2 werden kurz diskutiert.
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  • 5
    ISSN: 0044-2313
    Keywords: Lithium [tris(trimethylsilyl)silyl]tellanide · DME ; covalent radius of DME complexed Li ; [tris(trimethylsilyl)silyl]tellane ; methyl-[tris(trimethylsilyl)silyl]tellane ; bis[tris(trimethylsilyl)silyl]ditellane ; Te—H bond ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Derivatives of Molecular Compounds. IV Synthesis, Structure, and Reactivity of Lithium [Tris(trimethylsilyl)silyl]tellanide · DMELithium tris(trimethylsilyl)silanide · 1,5 DME [3] and tellurium react in 1,2-dimethoxyethane to give colourless lithium [tris(trimethylsilyl)silyl]tellanide · DME (1). An X-ray structure determination {-150 · 3·C; P21/c; a = 1346.6(4); b = 1497.0(4); c = 1274.5(3) pm; β = 99.22(2)·; Z = 2 dimers; R = 0.030} shows the compound to be dimeric forming a planar Li—Te—Li—Te ring with two tris(trimethylsilyl)silyl substituents in a trans position. Three-coordinate tellurium is bound to the central silicon of the tris(trimethylsilyl)silyl group and to two lithium atoms; the two remaining sites of each four-coordinate lithium are occupied by the chelate ligand DME {Li—Te 278 and 284; Si—Te 250; Li—O 200 pm (2X); Te—Li—Te 105°; Li—Te—Li 75°; O—Li—O 84°}. The covalent radius of 154 pm as determined for the DME-complexed lithium in tellanide 1 is within the range of 155 ± 3 pm, also characteristic for similar compounds. In typical reactions of the tellanide 1 [tris(trimethylsilyl)silyl]tellane (2), methyl-[tris(trimethylsilyl)silyl]tellane (4) and bis[tris(trimethylsilyl)silyl]ditellane (5) are formed.
    Notes: Lithium-tris(trimethylsilyl)silanid · 1,5 DME [3] reagiert mit Tellur in 1,2-Dimethoxyethan zu farblosem Lithium-[tris(trimethylsilyl)silyi]tellanid · DME (1). Nach der Röntgenstrukturanalyse {-150 ± 3°C; P21/c; a = 1346,6(4); b = 1497,0(4); c = 1274,5(3) pm; β = 99,22(2)°; Z = 2 Dimere; R = 0,030} ist Verbindung 1 im Festkörper dimer; die beiden Tris(trimethylsilyl)silyl-Gruppen sind am planaren Li—Te—Li—Te-Ring trans-ständig zueinander angeordnet. Tellur erreicht durch Bindung an zwei Lithium und ein Silicium die Koordinationszahl 3, Lithium durch Bindung an zwei Tellur und den Chelatliganden DME die Koordinationszahl 4 {Li—Te 278 und 284; Si—Te 250; Li—O 200 pm (2X); Te—Li—Te 105°, Li—Te—Li 75°; O—Li—O 84°}. Der hier zu 154 pm ermittelte kovalente Radius des DME-komplexierten Lithiumatoms fällt in den auch für andere Verbindungen typischen Bereich von 155 ± 3 pm. Charakteristische Umsetzungen des Tellanids 1 führen zu [Tris(trimethylsilyl)silyl]tellan (2), Methyl-[tris(trimethylsilyl)silyl]tellan (4) und Bis[tris(trimethylsilyl)silyl]ditellan (5).
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1646-1646 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Derivatives of Molecular Compounds. V. Synthesis and Structure of Hexakis{lithium-[tris(trimethylsilyl)silyl]tellanide} - Cyclopentane (1/1).Lithium [tris(trimethylsilyl)silyl]tellanide - DME (1/1) [1 b] prepared from lithium tris(trimethylsilyl)silanide - DME (2/3) [3] and tellurium, reacts with hydrogen chloride in toluene to form [tris(trimethylsilyl)silyl]tellane (1) [1 b]. Subsequent metalation of this compound with lithium n-butanide gives lithium [tris(trimethylsilyl)silyl]tellanide (2) free of coordinating solvent. Pale yellow crystals are obtained from cyclopentane solution. An X-ray structure determination {P1; a = 1 558.5(7); b = 1 598.4(8); c = 1 643.5(6) pm; α = 117.64(4); β = 91.63(3); γ = 117.19(3)°; Z = 1; R = 0.032} shows them to be the (1/1) packing complex (2′) of hexakis{lithium-[tris(trimethylsilyl)silyl]tellanide} and disordered cyclopentane molecules  - {Li—Te—Si[Si(CH3)3]3}6 · C5H10.
    Notes: Das aus Lithium-tris(trimethylsilyl)silanid - DME (2/3)1,2-Dimethoxyethan (DME); 1,4,7-Trimethyl-1,4,7-triaza-cyclo-nonan (TACN); Bis[2-(dimethylamino)ethyl]-methylamin (PMDTA); Tetrahydrofuran (THF); 1,4,7,10-Tetraoxa-cyclo-dodecan ([12]Krone-4); 2,4,6-Trimethylphenyl (Mes); 1,2-Bis(dimethylamino)ethan (TMEDA); Tetramethylsilan (TMS); Octamethyl-cyclo-tetrasiloxan (OMCT); Lösungsmittel (L.M.). [3] und Tellur leicht zugängliche, farblose dimere Lithium-[tris(trimethylsilyl)silyl]tellanid - DME (1/1) [1 b] reagiert mit Chlorwasserstoff in Toluol zu [Tris(trimethylsilyl)silyl]tellan (1); hieraus erhält man mit Lithium-n-butanid donorsolvens-freies Lithium-[tris(trimethylsilyl)silyl]tellanid (2). Wie eine Röntgenstrukturanalyse an den blaßgelben, aus Cyclopentan-Lösung isolierten Kristallen {P1; a = 1 558,5(7); b = 1 598,4(8); c = 1 643,5(6) pm; α = 117,64(4); β = 91,63(3); γ = 117,19(3)°; Z = 1; R = 0,032} zeigt, liegt Verbindung 2 im Festkörper hexamer vor; mit den in Hohlräumen der Struktur eingeschlossenen, fehlgeordneten Cyclopentan-Molekülen entsteht ein 1/1-Packungskomplex [11] der Zusammensetzung {Li—Te—Si[Si(CH3)3]3}6 · C5H10 (2′).Das Hexamer weist zwei aus Lithium- und tris(trimethylsilyl)silyl-substituierten Telluratomen in alternierender Abfolge aufgebaute, schwach gewellte sechsgliedrige Ringe mit Sesselkonformation auf, die über ein Inversionszentrum zu einem verzerrt hexagonalen Prisma verknüpft sind. Die endocyclischen Winkel in den sechs- und viergliedrigen Ringen dieses Polyeders variieren zwischen 102 und 126° bzw. 73 und 83° am vierfach koordinierten Tellur sowie zwischen 112 und 137° bzw. 96 und 106° am dreifach koordinierten Lithium. Einen signifikanten Unterschied beobachtet man auch zwischen den zu 273 bzw. 280 pm gemittelten basalen und axialen Li—Te-Abständen.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1455-1466 
    ISSN: 0044-2313
    Keywords: Tris(trimethylsilyl)methyl-derivatives, Lithium, Aluminium, Gallium, Indium ; spectra ; X-ray Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Base-free Tris(trimethylsilyl)methyl Derivatives of Lithium, Aluminium, Gallium, and IndiumBase-free LiR* (R*=-C(SiMe3)3) has been prepared from R*Cl and Li-metal in toluene at 85-90°C and used to synthesize the metallanes R*MMe2 with M = Al, Ga and In, respectively. The NMR (1H, 13C, 29Si) and the vibrational spectra of these trisyl compounds have been discussed.AlCl3 and LiR*(ratio 1 : 1) forms the metallate metallate Li[R*AlCl3]. The triclinic unit cell (space group P1) consists of a centrosymmetric assoziate, formed by four Li[R*AlCl3]- units with Al—Cl…Li bridges, two pairs of Li-atoms differing in their chlorine-coordination and two disordered toluene molecules, inserted in the crystal lattice (R1wR2 =0,0444/0,1072).The reaction of GaCl3 with LiR* (I :1) gives the unusual sesquichloride (R*Ga(Cl1,33)Me0,67)3 in moderate yield. The X-ray structure determination shows a Ga3Cl3-skeleton with chairconformation and disordered, terminal gallium ligands (R1/wR2= 0,0646/0,2270).
    Notes: Basefreies LiR* (R*=-C(SiMe3)3) wurde aus R*Cl und Lithiummetall in Toluol bei 85-90°C erhalten und zur Darstellung der Dimethylmetallane R*MMe2 mit M = Al, Ga, In verwendet, die durch NMR- (1H, 13C, 29Si) und Schwingungsspektren (Raman, IR) charakterisiert werden.AlCl3 und LiR* (Molverhältnis 1 : 1) bilden das Metallat Li[R*AlCl3]. Die trikline Einheitszelle (Raumgruppe P1) enthält ein zentrosymmetrisches, über Al—Cl … Li—Brücken gebildetes Assoziat aus vier Li[R*AlCl3]-Einheiten, mit zwei paarweise unterschiedlich von Chlor koordinierten Li-Atomen sowie zwei fehlgeordnete Toluolmoleküle (R1/ wR2 = 0,0444/0,1072).Die Reaktion von GaCl3 mit LiR* (1 : 1) in Toluol führt in mäßiger Ausbeute zum ungewöhnlichen Sesquichlorid (R*Ga(Cl1,33)Me0,67)3. Die Röntgenstrukturanalyse zeigt ein sesselförmig gewelltes Ga3Cl3-Sechsringgerüst und fehlgeordnete, terminale Liganden am Galliumatom (R1/ wR2 = 0,0646/0,2270).Li[R*AlCl3]. The triclinic unit cell (space group P1) consists of a centrosymmetric assoziate, formed by four Li[R*AlCl3]-units with Al-Cl … Li bridges, two pairs of Li-atoms differing in their chlorine-coordination and two disordered toluene molecules, inserted in the crystal lattice (R1/wR2 = 0,0444/0,1072).The reaction of GaCl3 with LiR* (1 : 1) gives the unusual sesquichloride (R*Ga(Cl1,33)Me0,67)3 in moderate yield. The X-ray structure determination shows a Ga3Cl3-skeleton with chairconformation and disordered, terminal gallium ligands (R1/wR2 = 0,0646/0,2270).
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1168-1174 
    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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  • 10
    Publication Date: 1993-09-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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