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  • 11
    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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  • 12
    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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  • 13
    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.
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  • 14
    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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  • 15
    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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  • 16
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: AgCo3H2(AsO4)3 and AgZn3H2(AsO4)3. Preparation and Crystal Structure. Another New Structure Type of an ArsenateAgCo3H2(AsO4)3 (1) and AgZn3H2(AsO4)3 (2) were prepared by heating of As2O5, AgNO3, CoSO4 · 7H2O, ZnSO4 · 7H2O, respectively, and water in a sealed tube at 300°C and investigated with X-rays. Both compounds are isotypic and crystallize in the monoclinic space group C2/c with 4 formula units per cell. The lattice parameters are (1): a = 1215.9(6), b = 1243.8(7), c = 678.2(3) pm, β = 113.16(3)° (2): a = 1216.9(2), b = 1249.5(3), c = 675.5(1) pm, β = 112.77(1)°. The structure contains chains of edge-shared CoO6 or ZnO6 octahedra, respectively, which are connected by AsO4 tetrahedra and silver oxygen ribbons with square planar coordinated silver forming a framework. Based on the charge balances derived from the geometrical data and the IR spectra the occurence of hydrogen bonds is discussed.
    Notes: AgCo3H2(AsO4)3 (1) und AgZn3H2(AsO4)3 (2) wurden durch Erhitzen eines Gemisches von As2O5, AgNO3, CoSO4 · 7H2O bzw. ZnSO4 · 7H2O und Wasser auf 300°C im Autoklaven dargestellt und röntgenographisch untersucht. Beide Verbindungen sind isotyp und kristallisieren in der monoklinen Raumgruppe C2/c mit 4 Formeleinheiten in der Elementarzelle. Die Gitterkonstanten sind: (1) a = 1215,9(6), b = 1243,8(7), c = 678,2(3) pm, β = 113,16(3)° (2) a = 1216,9(2), b = 1249,5(3), c = 675,5(1) pm,β = 112,77(1)°. Die Struktur enthält Ketten aus kantenverknüpften CoO6- bzw. ZnO6-Oktaedern, welche über AsO4-Tetraeder, sowie über Silber-Sauerstoff-Bänder mit quadratisch-planar koordiniertem Silber zu einem Gerüst verknüpft sind. Anhand der aus den geometrischen Daten berechneten Ladungsbilanzen und der IR-Spektren wird das Auftreten von Wasserstoffbrücken diskutiert.
    Additional Material: 3 Ill.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 491 (1982), S. 266-270 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N-Phenylmercury-N,N-bis(phosphoric diphenylester)imideSynthesis, properties, and structure of the title compound are described.
    Notes: Darstellung, Eigenschaften und Struktur der Titelverbindung werden beschrieben.
    Additional Material: 1 Ill.
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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 486 (1982), S. 187-192 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structure and Reactions of Phosphoric tris(N-dichlorophosphino-N-methylamide). Phosphoric tris(N-phenylchlorophosphino-N-methylamide)The X-ray structural analysis of phosphoric tris(N-dichlorophosphino-N-methylamide), I, is reported. Synthesis, properties and nmr data of phosphoric tris(N-phenylchlorophosphino-N-methylamide), III, are described.
    Notes: Es wird die Röntgenstrukturanalyse von Phosphorsäure-tris(N-dichlorphosphino-N-methylamid), I, mitgeteilt. Die Synthese, Eigenschaften und NMR-Daten von Phosphorsäure-tris(N-phenylchlorphosphino-N-methylamid), III, sind beschrieben.
    Additional Material: 1 Ill.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 504 (1983), S. 67-76 
    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.
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  • 20
    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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