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  • 1985-1989  (10)
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  • 1
    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.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 7-12 
    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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 534 (1986), S. 13-18 
    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.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 567 (1988), S. 39-47 
    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.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 521 (1985), S. 153-160 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Cyclic and Bicyclic Systems Made of Phosphorus, Carbon, and SulfurBy reaction of P4S10 with tertiary alkyl amines dialkylammonium salts of 3, 6- dialkyl1-2, 5-dithioxo-2λ5, 5°5-[1.4.2.5]dithiadiphosphorinan-2, 5-dithiols (V) are obtained. By pyrolysis the 3,6-dialkyl-2, 5, 7-trithia-1, 4-diphosphabicyclo[2.2.1] heptane-1,4-disulfides are formed (VIII). The result of an X-ray structural analysis of 3,6-di-isopropyl1-2,5,7-trithia-1,4-diphosphabicyclo [2.2.1]heptane-1,4-disulfide (VIIIc) is reported.
    Notes: Durch Umsetzung von P4S10 mit tertiären Alkylaminen werden Dialkylammonizumsalze von 3, 6-Dialkyl-2, 5-dithioxo-2λ5-[1.4.2.5]dithiadiphosphorinan-2,5-dithiolen (V) erhalten. Durch Pyrolyse entstehen daraus 3,6-Dialkyl-2,5, 7-trithia-1, 4-diphosphabicyclo[2.2.1]heptan-1, 4-disulfide (VIII). Von 3, 6-Di-isopropyl-2,5, 7-trithia-1,4-diphosphabicyclo[2.2.1]-heptan-1, 4-disulfid (VIIIc) wird das Ergebnis der Röntgenstrukturanalyse mitgeteilt.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 536 (1986), S. 129-136 
    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.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 530 (1985), S. 29-42 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Lithium Tris(trimethylsilyl)silanide · 1,5 DMELithium tris(trimethylsilyl)silanide · 1,5 DME 2a synthesized from tetrakis(trimethylsilyl)silane 1 [6] and methyllithium in 1,2-dimethoxyethane, crystallizes in the monoclinic space group P21/c with following dimensions of the unit cell determined at a temperature of measurement of -120 ± 2°C: a = 1 072.9(3); b = 1 408.3(4); c = 1 775.1(5) pm; β = 107.74(2)°; 4 formula units (Z = 2). An X-ray structure determination (Rw = 0.040) shows the compound to be built up from two [lithium tris(trimethylsilyl)silanide] moieties which are connected via a bridging DME molecule. Two remaining sites of each four-coordinate lithium atom are occupied by a chelating DME ligand. The Li—Si distance of 263 pm is considerably longer than the sum of covalent radii; further characteristic mean bond lengths and angles are: Si—Si 234, Li—O 200, O—C 144, OċO (biß) 264 pm; Si—Si—Si 104°, Li—Si—Si 107° to 126°; O—Li—O (inside the chelate ring) 83°. Unfortunately, di(tert-butyl)bis(trimethylsilyl)silane 17 prepared from di(tert-butyl)dichlorsilane 15, chlorotrimethylsilane and lithium, does not react with alkyllithium compounds to give the analogous silanide.
    Notes: Das aus Tetrakis(trimethylsilyl)silan 1 [6] und Lithiummethyl in 1,2-Dimethoxyethan1,2-Dimethoxyethan (DME); Tetrahydrofuran (THF); 1,2-Bis(dimethylamino)methan (TMEDA); Octamethylcyclotetrasiloxan (OMCT) zugängliche Lithium-tris(trimethylsilyl)silanid · 1,5 DME 2a kristallisiert monoklin in der Raumgruppe P21/c mit folgenden, bei einer Meßtemperatur von -120 ± 2°C bestimmten Parametern der Elementarzelle: a = 1 072,9(3); b = 1 408,3(4); c = 1 775,1(5) pm; β = 107,74(2)°; 4 Formeleinheiten (Z = 2). Nach den Ergebnissen der Röntgenstrukturanalyse (Rw = 0,040) baut sich die Verbindung aus zwei [Lithium-tris(trimethylsilyl)silanid]-Einheiten auf, die über ein DME-Molekül verbunden und deren vierfach koordinierte Lithiumatome von je einem weiteren DME-Liganden chelatartig umgeben sind. Mit 263 pm ist der Li—Si-Abstand wesentlich länger als die Summe der kovalenten Radien; weitere charakteristische mittlere Bindungslängen und -winkel sind: Si—Si 234, Li—O 200, O—C 144, OċO (Biß) 264 pm; Si—Si—Si 104°, Li—Si—Si 107° bis 126°, O—Li—O (im Chelatring) 83°. Das aus Di(tert-butyl)dichlorsilan 15, Chlortrimethylsilan und Lithium dargestellte Di(tert-butyl)bis(trimethylsilyl)silan 17 konnte bisher nicht in das analoge Silanid überführt werden.
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  • 8
    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 AgCu3Cu(AsO4)3 and its Structural Relations to AgCo3H2(AsO4)3 and AgZn3H2 (AsO4)3The compound AgCu3Cu(AsO4)3 was synthesized and investigated by X-rays. It crystallizes in the monoclinic space group C2/c with a = 1 212.7(2), b = 1 249.0(2), c = 727.8(1) pm, β = 117.94(1)°, Z = 4. The structure is closely related to the structures of AgCo3H2(AsO4)3 and AgZn3H2(AsO4)3. Only two hydrogen atoms are replaced by an additional copper atom forming a copper coordination square instead of two hydrogen bridges. The remaining copper atoms are sixfold coordinated with the generally observed Jahn-Teller distortion. Whereas in AgCo3H2(AsO4)3 and AgZn3H2(AsO4)3 silver has a (4+4) coordination, it is in this compound distinctly eightfold coordinated.
    Notes: Die Verbindung AgCu3Cu(AsO4)3 wurde synthetisiert und röntgenographisch untersucht. Sie kristallisiert in der monoklinen Raumgruppe C2/c mit a = 1 212,7(2), b = 1 249,0(2), c = 727,8(1) pm, β = 117,94(1)°, Z = 4. Die Struktur weist eine enge Verwandtschaft mit den Strukturen von AgCo3H2(AsO4)3 und AgZn3H2(AsO4)3 auf. Es sind hier lediglich zwei Wasserstoff-Atome durch ein zusätzliches Kupfer-Atom ersetzt, so daß anstelle zweier Wasserstoff-Brücken ein Kupfer-Quadrat eingebaut ist. Die anderen Kupfer-Atome sind sechsfach koordiniert mit der allgemein beobachteten Jahn-Teller-Verzerrung. Während beim AgCo3H2(AsO4)3 bzw. AgZn3H2(AsO4)3 Silber eine (4+4)-Koordination besitzt, liegt es hier in einer deutlichen Achterkoordination vor.
    Additional Material: 2 Ill.
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  • 9
    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.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 548 (1987), S. 63-75 
    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.
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