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  • 1
    Electronic Resource
    Electronic Resource
    Die Kristall- und Molekülstruktur von 2-Amino-2,4,4,6,6-pentafluor-1,3,5,2λ5,4λ5,6λ5-triazatriphosphorin (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 2934-2940 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of 2-Amino 2,4,4,6,6,-pentafluoro-1,3,5,2λ5, 4λ5, 6λ5- triazatriphosphorineThe crystal structure of the title compound 1 has been determined by direct methods from single crystal X-ray data and has been refined to R = 0.038 for 1465 reflections. The compound crystallizes in the monoclinic space group P21/c. The molecule forms a slightly puckered six-membered (P—N)3 ring. The endocyclic P—N bond lengths are significantly different (mean: 1.565 Å). The mean P—F bond length is 1.521 Å, the P—Namine bond length is 1.601 Å. The molecules are connected as layers through N—H⃛N hydrogen bonds.
    Notes: Die Struktur der Titelverbindung 1 wurde aus Diffraktometer-Einkristalldaten nach direkten Methoden bestimmt und für 1465 Reflexe zu einem R-Wert von 3.8% verfeinert. Die Verbindung kristallisiert monoklin in der Raumgruppe P21/c mit den Gitterkonstanten a = 7.958 Å, b = 5.222 Å, c = 19.297 Å, β = 101.24° Z = 4. Der P—N-Sechsring ist schwach gewellt. Die endocyclischen P—N-Abstände weisen signifikante Unterschiede auf (Einzelwerte: 1.551⃛1.586 Å, Mittelwert: 1.565 Å). Der Mittelwert der P—F-Bindungslängen beträgt 1.521 Å, die Länge der P—NAmin-Bindung ist 1.601 Å. Die Moleküle sind schichtartig über N—H⃛N-Wasserstoffbrücken verknüpft.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080913
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  • 2
    Electronic Resource
    Electronic Resource
    Die Kristall-und Molekülstruktur von 4,4,6,6-Tetrafluor-1,3,5,2λ5,4λ5,6λ5-triazatriphosphorin-2,2-diamin (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 2622-2627 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of 4,4,6,6-Tetrafluoro-1,3,5,2λ5,4λ5,6λ5-triazatriphosphorine-2,2-diamineThe crystal structure of the geminal isomer of N3P3F4(NH2)2 (3) was determined by X-ray analysis and was refined to R = 0.035. Crystals of the compound are orthorhombic, space group Pnma. The six-membered (P—N)3 ring is planar within the limits of error. In the (NH2)2 P—N—P(F2) segment the P—N bond lengths are 1.597 and 1.524Å with the shorter one on the side of the PF2 group. In the (F2)P—N—P(F2) segment the P—N bond length is 1.564 Å. The mean bond lengths in each P—N—P segment are nearly equal. The mean values for the P—F and P—Namine bond lengths were found to be 1.532 and 1.602 Å, respectively. The endocyclic angles are: N—P—N 110.4°, 120.5°; P—N—P 125.7°, 117.2°.
    Notes: Die Struktur des geminalen N3P3F4(NH2)2 (3) wurde aus Röntgenbeugungsdaten bestimmt und zu einem R-Wert von 3.5% verfeinert. Die Verbindung kristallisiert orthorhombisch in der Raumgruppe Pnma. Der (P—N)3-Ring ist innerhalb der Fehlergrenzen planar. Die P—N-Abstände betragen im (NH2)2 P—N—P(F2)-Segment 1.597 und 1.524 Å mit dem kürzeren Abstand auf der Seite der PF2-Gruppe. Im (F2)P—N—P(F2)-Segment ergibt sich die P—N-Bindungslänge zu 1.564 Å. Damit sind die Mittelwerte der Bindungslängen in jedem P—N—P-Segment nahezu gleich groß. Die Mittelwerte für die P—F- und die P—NAmin-Bindungslängen betragen 1.532 bzw. 1.602 Å. Die N—P—N-Winkel im Ring wurden zu 110.4° und 120.5°, die P—N—P-Winkel zu 125.7° und 117.2° beobachtet.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19761090733
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  • 3
    Electronic Resource
    Electronic Resource
    S3N2-Ringe mit fluorhaltigen Substituenten (1976)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 109 (1976), S. 1358-1361 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: S3N2-Rings with Fluorine Containing SubstituentsFrom the tin compound 1 and SOF2 the five-membered sulfur-nitrogen oxide 2 was prepared. 2 reacts with FSO2N=S=O, CF3SO2N=S=O, as well as with CF3SO2N=C=O and n-C4F9SO2NSO to yield the 1-sulfonylimino-1λ4,2,4λ4,3,5-trithiadiazoles 3,4 and 5 under evolution of SO2 as well as CO2. The X-ray structure analysis of 3 is reported. CH3SO2NSO, CF3S(O)NSO, and (CH3)3SiNSO react with 2 to form only sulfur and S4N4. In 1 the methyl-groups can be exchanged for chlorine atoms to give 7.
    Notes: Aus der Zinnverbindung 1 wurde mit SOF2 ein fünfgliedriges Schwefel-Stickstoff-Oxid 2 hergestellt. 2 reagiert mit FSO2N=S=O, CF3SO2N=S=O bzw. CF3SO2N=C=O und n-C4F9SO2NSO zu den 1-Sulfonylimino 1λ42,4λ4,3,5-trithiadiazolen 3,4 und 5 unter SO2-Abspaltung. Die Röntgenstrukturanalyse von 3 wird mitgeteilt. CH3SO2NSO, CF3S(O)NSO und (CH3)3SiNSO ergeben mit 2 lediglich Schwefel und S4N4. In 1 lassen sich die Methylgruppen mit SnCl4 gegen Chloratome unter Bildung von 7 austauschen.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19761090417
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  • 4
    Electronic Resource
    Electronic Resource
    The Crystal Structure of Bi8(AlCl4)2 and the Crystal Structure, Conductivity, and Theoretical Band Structure of Bi6Cl7 and Related Subvalent Bismuth Halides (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1219-1226 
    Details
    ISSN: 0009-2940
    Keywords: Bismuth subhalides ; Band structure and electrical conductivity of Bi6Cl7 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The methods of preparation for Bi8(AlCl4)2 and Bi6Cl7 have been improved and the single crystal structures for these cluster compounds re-investigated and re-interpreted. In addition, conductivity measurements and band structure calculations using the tight-binding approximation have been performed on Bi6Cl7 and related subvalent bismuth halides. - Bi8(AlCl4)2 consists of isolated AlCl4- anions and rather undistored square-antiprismatic Bi82+ clusters with an average Bi-Bi distance of 3.10 Å. Relatively short intercluster Bi-Bi contacts of 3.90 Å suggest weak bonding interactions between the Bi82+ units. In contrast, the structure determination of Bi6Cl7 implies that this structure should be regarded as being composed of discrete Bi95+ clusters and a polymeric BiIII-Cl anionic lattice including infinite, distorted α1[Bi2Cl24+] chains. According to the experimental and theoretical results, the Bi6X7 (X = Cl, Br) family of subvalent bismuth halide compounds are anisotropic semiconductors along the crystallographic c axis. The conductivity is mediated by the onedimensional α1[Bi2Cl24+] chains. These are interconnected with the Bi95+ clusters, which are acting as electron reservoirs. The related BiX (X = Br, I) family of subvalent bismuth halides are shown to be anisotropic semiconductors in the crystallographic b direction.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291013
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  • 5
    Electronic Resource
    Electronic Resource
    Reactive E=C [p-p] π Systems, 46Part 45: Ref. Syntheses and X-ray Crystal-Structure Analyses of Trifluoromethyl-Substituted Ketiminodiselanes, Selenoamides and SelenoacrylamidesDedicated to Professor Peter Sartori on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 913-922 
    Details
    ISSN: 0009-2940
    Keywords: Selenium ; Fluorine ; Amides ; Cleavage reactions ; Cycloadditions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(trifluoromethylketiminoalkyl)diselanes [SeC(=NR)CF3]2 (6) [R = Me (a), iPr (b), tBu (c)] have been prepared in high yields (55-70%) by reaction of the diselane (SeC2F5)2 (2) with RNH2. However, the analogous reaction of 2 with secondary amines, R2NH, results in the cleavage of the Se-Se bond and leads to the N,N-dialkyl-2,2,2-trifluoroselenoacetamides Se=C(NR2)CF3 (7) [R = Me (a), iPr (b)]. Cleavage of 6a-6c with Me3SnH affords the selenoamides Se=C(NHR)CF3 (9) and the corresponding stannylselanes Me3SnSeC(=NR)CF3 (10) [R = Me(a), iPr (b), tBu (c)]. Selenoamides 7 and 9 can also be prepared from pentafluoroethylselenol HSeC2F5 (3), Se=C(F)CF3, (1) or its polymer [SeC(F)CF3]n (4) and primary or secondary amines. N,N-dialkyl-2-methyl-3-fluoro-4,4,4-trifluoroselenoacrylamides Se=C(NR2)C(Me)=C(F)CF3[R = Et (13a), iPr (13b)] are prepared in moderate yields under mild conditions by treating either trifluoromethylselenocarbonyl fluoride (1) or its polymer [SeC(F)CF3]n with 1-dialkylamino-1-propynes. The reaction proceeds by [2 + 2] cycloaddition and stereospecific electrocyclic ring-opening, yielding, with respect to the resulting C=C double bond, the E isomer as the only product. The molecular structures of 7b, 9a and 13b show the typical features of selenoamides with C(Se)-N bond shortening and C-Se bond elongation due to π interaction of the N lone pair with the C=Se double bond. The observed perpendicular orientation of the selenoamide and the alkene units of 13b prevents π delocalization.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300717
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  • 6
    Electronic Resource
    Electronic Resource
    Metallkomplexe unsymmetrisch überbrückter [N4]-Makrocyclen: Synthese, Struktur und Redoxverhalten (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 503-514 
    Details
    ISSN: 0009-2940
    Keywords: Cu, Ni, Co, Fe complexes ; Template synthesis ; Tetraaza macrocycles ; X-ray structure, H bridges, ID-coordination polymers ; Electrochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes of Unsymmetrically Bridged [N4] Macrocycles: Synthesis, Structure and Redox BehaviourMetal complexes M-5a (M = Cu, Ni, Co, Fe, and I-Fe11) of 6,13-Di(ethoxycarbonyl)-7,12-dimethyl-benzo[b]-1,4,8,11-tetraaza-cyclotetradeca-2,5,7,11,13-pentaene and the free ligand H2-5a have been synthesized. The crystals of Cu-5a · H2O and Ni-5a · H2O consist of planar complex molecules which are linked by H bridges between the water molecules and the peripheric ester groups to give 1D chains. The average M-N distances are equal for both complexes (Cu 1.928, Ni 1.924 Å), being unexpectedly large for the nickel complex. The redox properties of all the new compounds as well as some acetyl derivatives M-5b have been examined by cyclic voltammetry and compared with those of the previously reported symmetrically phenylene (M-4) and ethylene (M-6) bridged derivatives. All complexes give a reversible single electron reduction which clearly shows the increasing electron density around the central atom in the order M-4 〈 M-5 〈 M-6. Like the carbonyl substituted tetraazaannulenes M-4 the copper complexes Cu-5 give two, the cobalt complexes Co-5 three, and the iron complex Fe-5a probably four reversible single electron oxidations. They can be attributed to the species [MIIIL-II]+, [MIILo]2+, [MIIILo]3+, and [FeIVLo]4+ with Lo being a “non innocent” neutral 1,2-quinodiimine ligand. Very surprisingly, since in contrast to Ni-4 and Ni-6, the nickel complexes Ni-5 gave no reversible oxidation.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280512
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  • 7
    Electronic Resource
    Electronic Resource
    Reactive E=C [p-p]π Systems, 45[Part 44: See ref.[1].]. 1-Aza-3,4-diphospholenes by [3 + 2] Cycloaddition of 2-(Diisopropylamino)phosphaethyne to Diazo Derivatives R1R2C=N2Dedicated to Professor Max Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1271-1274 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkyne ; [3 + 2] Cycloaddition ; 1-Aza-3,4-diphospholenes ; Diphosphiranes ; 1-Aza-3,4-diphospholes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the (diisopropylamino)phosphaethyne (1) with diazo compounds of the type R1R2C=N2 (2a-2c) unexpectedly leads in high yields (60-90%) to the 1-aza-3,4-diphospholene derivatives 3a-3c, a new class of heterocycles. NMR investigations of the analogous reaction of 1 with diazocyclopentadiene 2d show that the multi-step formation of 3a-3c proceeds via the 1-aza-3,4-diphospholes 6a-6d as intermediates.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291020
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  • 8
    Electronic Resource
    Electronic Resource
    Kristallstruktur des N-Nitrosodimethylamins (1975)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 108 (1975), S. 1130-1137 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of N-NitrosodimethylamineThe crystal structure of the title compound has been determined from single crystal low temperature X-ray counter data collected at - 130°C. Bond lengths in the exactly planar molecule were found to be N — N 1.320(6), N — O 1.260 (6), C — N 1.461 (7) and 1.465 (7) Å. The bonding in the molecule is significantly closer to the polar structure compared to the free molecule in the gas phase, this being stabilised by intermolecular π interactions perpendicular to the planes of the molecules.
    Notes: Die Struktur des festen N-Nitrosodimethylamins bei - 130°C wurde durch Röntgenstruktur-analyse bestimmt. Das Molekül ist im Kristall exakt planar. Die Bindungslängen bei - 130°C sind: N — N 1.320(6), N — O 1.260(6), C — N 1.461(7) und 1.465(7) Å. Senkrecht zu den Molekülebenen verlaufende intermolekulare π-Wechselwirkungen stabilisieren einen höheren Anteil der polaren Struktur am Bindungszustand gegenüber dem freien Molekül der Gasphase.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19751080419
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  • 9
    Electronic Resource
    Electronic Resource
    Die Kristall- und Molekülstruktur von [Bis(trimethylsilyl)amino]-bis(trimethylsilylimino)phosphoran (1977)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 110 (1977), S. 3183-3189 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal and Molecular Structure of [Bis(trimethylsilyl)amino]-bis(trimethylsilylimino)phosphoraneThe crystal structure of the title compound 1 was determined from single crystal X-ray data (measured at +18 and -130°C) and was refined to R = 0.043 (-130°C). The compound crystallizes in the monoclinic space group C2/c. Comparison of bond lengths in 1 at the two temperatures demonstrates the necessity of a correction for shortening due to thermal motion for the SiR3-groups (R = methyl). The planar threefold nitrogen coordination of the phosphorus seems to favor the assumption of pπ-pπ-bonds. The P-Nimine and P-Namine bond lengths were found to be 1.515 and 1.638 Å, respectively; Nimine-Si 1.703, Namine-Si 1.787 Å, angle P = N-Si 146.8° (all values for -130°C).
    Notes: Die Struktur der Titelverbindung 1 wurde aus bei + 18 und - 130°C ermittelten Diffraktometer-Einkristalldaten bestimmt und zu einem R-Wert von 4.3% (-130°C) verfeinert. Die Verbindung kristallisiert monoklin in der Raumgruppe C2/c. Z = 4. Ein Vergleich der Bindungslängen in 1 bei den verschiedenen Temperaturen zeigt für die endständigen Trimethylsilylgruppen die Notwendigkeit einer Korrektur der durch thermische Schwingungen scheinbar verkürzten Abstände. Das zentrale Phosphoratom weist eine planare dreifache Koordination von Stickstoffatomen auf. Bindungslängen und die Symmetrie des Moleküls deuten auf die Existenz von pπ-pπ-Bindungen zwischen Phosphor und Stickstoff hin. Der P-NImin-Abstand beträgt 1.515, der P-NAmin-Abstand 1.638 Å. Die NImin-Si- und NAmin-Si-Bindungslängen wurden zu 1.703 bzw. 1.787 Å beobachtet. Der P = N-Si-Winkel beträgt 146.8° (alle Werte für -130°C).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19771100924
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  • 10
    Electronic Resource
    Electronic Resource
    Trigonal planar koordinierter Schwefel(VI): Die Kristall- und Molekülstrukturen von (R3SiN)3S und (R3CN)3S (R=CH3) bei -130°C (1979)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 112 (1979), S. 1751-1755 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Planar Threefold Coordination of Sulfur(VI): Crystal and Molecular Structures of (R3SiN)3S and (R3CN)3S (R=CH3) at -130°CThe crystal structures of the title compounds were determined from single crystal X-ray data (measured at -130°C) and refined to unweighted R-values of 0.034 for (R3SiN)3S (1) and 0.047 for (R3CN)3S(2). 2 crystallizes in the triclinic space group P1 and 1 in the hexagonal space group P63/m. Both structures exhibit a planar threefold nitrogen coordination of the sulfur but the large coefficients of the temperature factors perpendicular to the SN3 planes in 1 and 2 might indicate a disorder due to small deviations from planarity. The S—N bond lengths were found to be 150.4 (1) and 151.5 pm (2, mean).
    Notes: Die Strukturen der Titelverbindungen wurden aus Diffraktometer-Einkristalldaten (gemessen bei -130°C) bestimmt und zu ungewichteten R-Werten von 0.034 für (R3SiN)3S )(1) und 0.047 für (R3CN)3S (2)verfeinert. 2 kristallisiert triklin, P1. Und 1 hexagonal, P63/m. In beiden Strukturen wird eine trigonal planare Koordination des zentralen Schwefelatoms beobachtet, doch deuten die relativ großen Koeffizienten der anisotropen Temperaturfaktoren senkrecht zu den SN3-Ebenen in 1 und 2 auf eine Fehlordnung als Folge geringer Abweichungen von der Planarität in den einzelnen Molekülen hin. Die S—N-Abstände betragen 150.4 pm (1) und 151.5 pm (2, Mittelwert).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19791120525
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