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  • 1
    Electronic Resource
    Electronic Resource
    Synthese und NMR-Spektren von λ5-Diphospheten Die Struktur des 2,4-Diphenyl-1,1,3,3-tetrakis(diethylamino)-1λ5,3λ5-diphosphetsProfessor Lothar Kolditz zum 60. Geburtstage gewidmet (1989)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 576 (1989), S. 81-98 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and NMR Spectra of λ5-Diphosphets. Structure of 2,4-Diphenyl-1,1,3,3-tetrakis (diethylamino)-1λ5, 3λ5-diphosphetePreparation, properties, and n.m.r. spectra of C2H5PF2[N(C2H5)2]2, CH2=PF[N(C2H5)2]2, and the diphosphetes {RC=P[N(C2H5)2]2}2 (R) = H (5a), CH3 [(5b)] are described. The λ5-diphosphete {HC=P(NR2)2}2 (R = CH3) reacts with BF3 · O(C2H5)2 to give which is transformed into by n-C4H9Li. The crystal and molecular structure of 2,4-diphenyl-1,3,3-tetrakis(diethylamino)-1λ5,3λ5-diphosphete 2 are reported and discussed.
    Notes: Darstellung, Eigenschaften und NMR-Spektren von C2H5PF2[N(C2H5)2]2, CH2=PF[N(C2H5)2]2 und der Diphosphete {RC=P[N(C2H5)2]2}2 (R = H )(5a), CH3 [(5b)] werden beschrieben. Das λ5-Diphosphet {HC=P(NR2)2}2 (R = CH3) reagiert mit BF3 · O(C2H5)2 zu das mit n-C4H9Li in übergeht. Die Kristall- und Molekülstruktur von 2,4-Diphenyl-1,1,3,3-tetrakis(diethylamino)-1λ5,3λ5-diphosphet 2 werden mitgeteilt und diskutiert.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19895760111
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  • 2
    Electronic Resource
    Electronic Resource
    Bemerkungen zur Synthese von Difluorphosphoranen n-Butyl-bis(dimethylamino)alkylidenphosphorane. Der Komplex {(CO)4FeC[OSi(CH3)3]CH=P(n-C4H9)[N(CH3)2]2} (1990)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 588 (1990), S. 147-166 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Remarks to the Synthesis of Difluorophosphoranes. n-Butyl-bis(dimethylamino)alkyliden-phosphoranes. Complex {(CO)4FeC[OSi(CH3)3]CH=P(n—C4H9) [N(CH3)2]2}Diethylamino-diethylaminosulfanyl-difluoro-i-butyl-phosphorane 3 is formed in the synthesis of bis(diethylamino)-difluoro-i-butyl-phosphorane from the corresponding phosphane by fluorination with SF4 as a by-product. Synthesis, NMR spectra, and reactions of n-butyl-bis(dimethylamino)alkylidene phosphoranes are reported. n-Butyl-bis(dimethylamino)-trimethylsilylmethylidenphosphorane, 17, reacts with Fe(CO)5 to give the tetracarbonyliron complex 19. The result of the X-ray structural analysis of 19 is reported and discussed.
    Notes: Diethylamino-diethylaminosulfanyl-difluor-i-butyl-phosphoran 3 entsteht als Nebenprodukt bei der Synthese von Bis(diethylamino)-difluor-i-butyl-phosphoran aus dem entsprechenden Phosphan durch Fluorierung mit SF4. Synthese, NMR-Spektren und Reaktionen von n-Butyl(bisdimethylamino)alkylidenphosphoranen werden berichtet. n-Butyl-bis(dimethylamino)-trimethylsilylmethylidenphosphoran, 17, reagiert mit Fe(CO)5 zu dem Tetracarbonyleisen-Komplex 19. Das Ergebnis der Röntgenstrukturanalyse von 19 wird mitgeteilt und diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19905880119
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  • 3
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur von Methylphosphoniumchlorid (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 536 (1986), S. 129-136 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structures of Methylphosphonium ChlorideThe reaction between methyldichlorophosphane and glycol in dichloromethane yields [CH3PH3]Cl and CH2[—OP(O)CH3(OCH2CH2Cl)]2. The molecular and crystal structure of [CH3PH3]Cl are reported.
    Notes: Bei der Umsetzung von Methyldichlorphosphan mit Glykol in Dichlormethan entstehen [CH3PH3]Cl und CH2[—OP(O)CH3(OCH2CH2Cl)]2. Die Molekül- und Kristallstruktur von [CH3PH3]Cl werden mitgeteilt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865360515
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  • 4
    Electronic Resource
    Electronic Resource
    Unsymmetrisch diphosphorsubstituierte Acetylene (1988)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 39-47 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Unsymmetrically Diphosphorus Substituted AcetylenesBis[bis(diethylamino)difluorophosphoranyl]acetylene, 4, reacts with an equimolar amount of BF3 · ether to give the phosphonium tetrafluoroborate 7 which is only stable at low temperatures. 7 is characterized by its n.m.r. spectra and the results of an X-ray analysis. With the double molar amount of BF3 · ether, 4 yields the diphosphonium bis(tetrafluoroborate) 8. Bis[bis(diethylamino)phosphanyl]acetylene is oxidized by tetrachloro-o-benzoquinone to give compound 6.
    Notes: Bis[bis(diethylamino)difluorphosphoranyl]acetylen, 4, bildet mit der äquimolaren Menge BF3 · Ether das nur bei niedrigen Temperaturen stabile Phosphonium-tetrafluoroborat 7, das durch seine NMR-Spektren und die Ergebnisse einer Röntgenstrukturanalyse charakterisiert wird. Mit der doppelt molaren Menge BF3 · Ether bildet 4 das Diphosphonium-bis(tetrafluoroborat) 8. Bis[bis(diethylamino)phosphanyl]acetylen wird von Tetrachlor-o-benzochinon zu Verbindung 6 oxidiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19885670105
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  • 5
    Electronic Resource
    Electronic Resource
    Darstellung und Struktur des N,N′ -DithioformylanilinsProfessor Josef Goubeau zum 85. Geburtstage am 31. März 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 7-12 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of N,N′-DithioformylanilineN,N′-dithioformylaniline was prepared by treating N,N′-dichlormethylaniline [1] with silicon disulfide [2]. The compound is characterized by the results of a X-ray structural analysis (RW = 0.030) as well as its nmr and vibration spectra. N,N′-dithioformylaniline crystallizes in the orthorhombic space group P21212 with a = 537.0(2); b = 745.7(3); c = 1111.5(4) pm; V = 445.1(3) · 106 pm3. The molecule consists of two planar parts; the angle between the plane of the aromatic ring and the plane of the N,N′-dithioformylamino group was determined to 87.7°.
    Notes: N,N′-Dithioformylanilin konnte durch Umsetzung von N,N′-Dichlormethylanilin [1] mit Siliciumdisulfid [2] dargestellt werden. Die Verbindung ist durch die Ergebnisse einer Röntgenstrukturanalyse (RW = 0,030) sowie ihre NMR- und Schwingungsspektren charakterisiert. N,N′-Dithioformylanilin kristallisiert orthorhombisch in der Raumgruppe P21212 mit Z = 2 und a = 537,0(2); b = 745,7(3); c = 1111,5(4) pm; V = 445,1(3) · 106 pm3. Das Molekül weist zwei planare Bauteile auf; der Winkel zwischen der Ebene des Aromaten und der durch die N,N′-Dithioformylaminogruppe gelegten Ebene wurde zu 87,7° bestimmt.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865340302
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  • 6
    Electronic Resource
    Electronic Resource
    Die Kristall- und MolekülStruktur des N,N′-DiformylanilinsProfessor Josef Goubeau zum 85. Geburtstage am 31. März 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 13-18 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of N,N′-DiformylanilineN,N′-diformylaniline crystallizes in the monoclinic space group P21/n with Z = 8 and a = 856.1(2), b = 1277.6(3), c = 1306.1(3) pm, β 92.29(2)°, V = 1427.4(5) · 106 pm3. As shown by X-ray structure determination (2642 symmetry independent reflections, RW = 0.034) the molecule exists in two enantiomeric forms. The molecular structure can be described by two planes; the angle between the plane of the aromatic ring and the plane of the N,N′-diformylamino group is 70.1 resp. 108.3°. The results are compared with those obtained for other derivats.
    Notes: N,N′-Diformylanilin kristallisiert monoklin in der Raumgruppe P21/n mit Z = 8 und a = 856,1(2); b = 1277,6(3); c = 1306,1(3) pm; β = 92,29(2)°; V = 1427,4(5) · 106 pm3. Nach den Ergebnissen der Röntgenstrukturanalyse (2642 symmetrieunabhängige Reflexe; RW = 0,034) existiert das Molekül in zwei enatiomeren Formen. Die Molekülstruktur kann durch zwei Ebenen beschrieben werden; der Winkel zwischen der Ebene des Aromaten und der durch die N,N′-Diformylaminogruppe gelegten Ebene beträgt 70,1 bzw. 108,3°. Die Ergebnisse werden mit denen anderer Derivate verglichen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865340303
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  • 7
    Electronic Resource
    Electronic Resource
    Acyl- und Alkylidenphosphane. XXVIII. Synthese und Struktur von 1,3-Dibenzyl- und 1,3-Diethyl-2,4-bis(phenylimino)-1,3-diphosphetanProfessor Josef Goubeau zum 85. Geburtstage am 31. März 1986 gewidmet (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 31-49 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acyl- and Alkylidenephosphines. XXVIII. Synthesis and Structure of 1,3-Dibenzyl- and 1,3-Diethyl-2,4-bis(phenylimino)-1,3-diphosphetaneCatalyzed by small amounts of solid sodium hydroxide, the adducts 1a and 1b formed from benzyl- or ethylbis(trimethylsilyl)phosphine and phenylisocyanate, react at +20°C slowly to give hexamethldisiloxane and oligomeric [(phenylimino)methylidene]phosphines. In different solvents the benzyl compound was found to exist only as a mixture of [N,N′-(E)/(Z)]-isomeric 2,4-bis-(phenylimino)-1,3-diphosphetanes 2a with their alkyl groups at the phosphorus atoms in trans position, whereas in case of the ethyl derivative 2b a second pair of [N,N′-(E)/(Z)]-isomeric dimers with their substituents in cis position and two trimeric forms (3b and 4b) could be detected in cyclopentane. [N,N′-(E)]-1r,3t-dibenzyl- (2a) and [N,N′-(E)]-1r,3t-diethyl-2,4-bis(phenylimino)-1,3-diphosphetane 2b isolated from 1,2-dimethoxyethane or cyclopentane, crystallize in the monoclinic space group P21/c or P21/n, resp., with following dimensions of the unit cell determined at temperatures of measurement of +20 ± 3°C/-130 ± 3°C: a = 2145.4(1)/569.3(1); b = 568.1(2)/719.1(2); c = 1960.2(2)/2042.6(4) pm; β 99.43(1)°/95.03(2)°; Z = (2+2) and 2, resp. X-ray structure determinations (Rw = 0.034/0.041) show both molecules to be centrosymmetric. Characteristic rounded bond lengths (pm) and angles (°) are: endocyclic P—C 185/184; C—P—C 82/81; P—C—P 98/99; exocyclic P—C 186/184; C=N l27/127; C=N—C 121/11.
    Notes: Unter der Katalyse von wenig festem Natriumhydroxid setzen sich die aus Benzyl- oder Ethylbis(trimethylsilyl)phosphan und Phenylisocyanat gebildeten Addukte 1a und 1b bei +20°C langsam zu Hexamethyldisiloxan und oligomeren [(Phenylimino)methyliden]phosphanen um. Während die Benzyl-Verbindung in unterschiedlichen Lösungsmitteln nur als Gemisch aus [N,N′-(E)]- und [N,N′-(Z)]-isomerem 2,4-Bis(phenylimino)-1,3-diphosphetan 2a mit den beiden Alkylgruppen an den Phosphoratomen in trans-Stellung vorliegt, findet man bei dem in Cyclopentan gelösten Ethyl-Derivat 2b ein weiteres [N,N′-(E)/(Z)]-isomeres Dimerenpaar mit zueinander cisständigen Substituenten sowie die beiden trimeren Formen 3b und 4b. Die aus 1,2-Dimethoxyethan oder Cyclopentan isolierten Verbindungen [N,N′-(E)]-1r,3t-Dibenzyl- (2a) und [N,N′-(E)]-1r,3t-Diethyl-2,4-bis(phenylimino)-1,3-diphosphetan 2b kristallisieren monoklin in der Raumgruppe P21/c bzw. P21/n mit folgenden, bei Meßtemperaturen von +20 ± 3°C/-130 ± 3°C bestimmten Abmessungen der Elementarzelle: a = 2145,4(1)/569,3(1); b = 568,1(2)/719,1(2); c = 1960,2(2)/2042,6(4) pm; β 99,43(1)°/95,03(2)°; Z = (2+2) bzw. 2. Nach den Ergebnissen von Röntgenstrukturanalysen (RW = 0,034/0,041) weisen die Moleküle Inversionszentren auf. Charakteristische gemittelte Bindungslängen (pm) und -winkel (°) sind: endocycl. P—C 185/184; C—P—C 82/81; P—C—P 98/99; exocycl. P—C 186/184; C=N 127/127; C=N—C 121/11.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865340306
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  • 8
    Electronic Resource
    Electronic Resource
    Bisphosphoranylacetylene und der Cobaltkomplex Co2(CO)6{[(C2H5)2N]2PF2C≡CPF2[N(C2H5)2]2} (1987)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 548 (1987), S. 63-75 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bisphosphoranylacetylenes and the Cobalt Complex Co2(CO)6{[(C2H5)2N]2PF2C≡CPF2[N(C2H5)2]2}Synthesis and properties of bis[difluorobis(diethylamino)phosphoranyl]acetylene, 2, bis(difluorodimorpholinophosphoranyl)acetylene, 4, and bis(trifluorodiethylaminophosphoranyl)-acetylene, 6, are described. With Co2(CO)8 2 forms the coordination compound hexacarbonyl-μ-η-bis-[difluorobis(diethylamino)phosphoranyl]acetylene-dicobalt(Co—Co), 7. The results of the X-ray structural analysis of 2 and 7 are reported.
    Notes: Synthese und Eigenschaften von Bis[difluorbis(diethylamino)phosphoranyl]acetylen, 2, Bis(difluordimorpholinophosphoranyl)acetylen, 4, und Bis(trifluordiethylaminophosphoranyl)acetylen, 6, werden beschrieben. Mit Co2(CO)8 bildet 2 die Komplexverbindung Hexacarbonyl-μ-η-bis[difluorbis(diethylamino)phosphoranyl]acetylen-dicobalt (Co—Co), 7. Von 2 und 7 werden die Ergebnisse der Röntgenstrukturanalyse mitgeteilt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19875480507
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  • 9
    Electronic Resource
    Electronic Resource
    Über Diazadiphosphetidine. III. N,N′-Diphosphoryl-diaza-λ3,λ3-diphosphetidineProfessor Werner Reif zum 60. Geburtstage am 24. September 1981 gewidmet. (1982)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 486 (1982), S. 177-186 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Diazadiphosphetidine. III. N,N′-Diphosphoryl Diaza-λ3,λ3-diphosphetidinesSynthesis, structure and mass spectrum of trans 1,3-bis(diethoxyphosphoryl)-2,4-bis(diethylamino)-1,3,2,4-diaza- λ3,λ3-diphosphetidine (I) are described. Furthermore the procedure for preparing bis(diethylamido)-phosphorous-(N-diethoxyphosphoryl)-imide (III) and 1,3-bis(diphenoxyphosphoryl)-2,4-bis(diethylamino)-1,3,2,4-diaza-λ3,λ3-diphosphetidine (VI) is presented. I, N-diethyl-N′N″-bis(diethoxyphosphoryl)-phosphorous triamide (II), III, VI and bis(diethylamido)-phosphorous(N-diphenoxyphosphoryl)-imide(VIII) are characterized by their nmr spectra.
    Notes: Synthese, Struktur und Massenspektrum von trans-1,3-Bis(diethoxyphosphoryl)-2,4-bis(diethylamino)-1,3,2,4-diaza-λ3,λ3-diphosphetidin (I) werden beschrieben. Weiter wird die Synthese von Bis(diethylamido)-phosphorigsäure-(N-diethoxyphosphoryl)-imid (III) und 1,3-Bis(diphenoxyphosphoryl)-2, 4-bis(diethylamino)-1,3,2,4-diaza-λ3,λ3-diphosphetidin (VI) mitgeteilt. I, N-Diethyl-N′,N″-bis(diethoxyphosphoryl)-phosphorigsäuretriamid (II), III, VI und Bis-(diethylamido)-phosphorigsäure-(N-diphenoxyphosphoryl)-imid (VIII) sind durch ihre Spektren charakterisiert.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19824860120
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  • 10
    Electronic Resource
    Electronic Resource
    Dimethylaminoalane, H3 - n Al[N(CH3)2]n, n = 1, 2, 3 Kristallstrukturen und Molekülspektren (1983)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 504 (1983), S. 67-76 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimethylaminoalanes, H3 - nAl[N(CH3)2]n, n = 1, 2, 3; Crystal Structures and Molecular SpectraThe X-ray crystal structure analyses of dimethylaminoalane (I), bis(dimethylamino)alane, and tris(dimethylamino)alane are reported and the molecular spectra of these compounds are discussed. I is trimeric and exists as sixmembered ring of a chair-conformation. II and III are dimeric and build up planar four-membered rings.
    Notes: Es werden die Röntgenstrukturanalysen von Dimethylaminoalan (I), Bis(dimethylamino)alan (II) und Tris(dimethylamino)alan (III) mitgeteilt und deren Molekülspektren diskutiert. I ist trimer und liegt als Sechsring in der Sesselform vor; II und III sind dimer und bilden planare Vierringe aus.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19835040909
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