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  • 1
    Electronic Resource
    Electronic Resource
    Syntheses of 3-Heteroaryl-2H-Azaphosphirene Tungsten Complexes (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 575-578 
    Details
    ISSN: 1434-1948
    Keywords: Phosphorus heterocycles ; 2H-Azaphosphirene complexes ; Carbene complexes ; Tungsten ; Cyclizations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The syntheses of 3-heteroaryl-substituted 2H-azaphosphirene pentacarbonyltungsten complexes are reported. The products were characterized by multinuclear NMR spectroscopy (1H, 13C, 15N, 31P, 183W); the structure of the 3-N-methylpyrryl-substituted 2H-azaphosphirene complex was determined by single-crystal X-ray structure analysis.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Syntheses, Structures, and Reactions of C-Methoxycarbonyl-Functionalized Small- and Medium-Sized P-Heterocycle Complexes (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 1567-1579 
    Details
    ISSN: 1434-1948
    Keywords: Phosphorus heterocycles ; 2H-Azaphosphirene complexes ; Water-soluble P ligands ; Tungsten ; Cyclizations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal ring-opening of [{2-bis(trimethylsilyl)methyl-3- phenyl-2H-azaphosphirene-ĸP}pentacarbonyltungsten(0)] (8a) in the presence of dimethyl acetylenedicarboxylate (DMAD) led to the 2,3-bifunctionalized 1H-phosphirene complex 9a and the 4-phenyl-substituted 2H-1,2-azaphosphole complex 10a, the latter as a by-product. If a small amount of benzonitrile was added, complex 10a was obtained as the main product, along with a small amount of the decomplexed 2H-1,2-azaphosphole 11, which could not be isolated. Reaction of complex 10a with elemental sulfur furnished the corresponding PV sulfide 13. When the ring-opening of complex 8a was performed in the presence of two equivalents of DMAD and two equivalents of dimethyl cyanamide, we obtained the 4-dimethylamino-substituted 2H-1,2-azaphosphole complex 10b, together with the diastereomeric Δ3-1,3,2-oxazaphospholene complexes 14a,b. On reaction of [{2-pentamethylcyclopentadienyl-3-phenyl-2H-azaphosphirene-ĸP}pentacarbonyltungsten(0)] (8b) and DMAD in toluene, the corresponding 1H-phosphirene complex 9b was only formed as a transient species and the P-coordinated P,C-cage compound 15 was the final product. Using benzonitrile as solvent, the 4-phenyl-substituted 2H-1,2-azaphosphole complex 10c was obtained, together with the 7-aza-1-phosphanorbornadiene complex 16, the latter through partial decomposition of 10c coupled with rearrangement and a Diels-Alder reaction; the ratio 10c/16 was found to depend strongly on the molar ratio of complex 8b to DMAD. A cycloaddition reaction of the 2,3-bifunctionalized 1H-phosphirene complex 9a with 2,3-dimethylbutadiene furnished the bicyclic phosphirane complex 19, along with a small amount of the noncoordinated bicyclic phosphirane 20. Reaction of complex 9a with diethylamine yielded the phosphirane complex 21 as a 1,2-addition product, the diorganophosphane complex 22 through ring-opening of 9a, and the 3,4-functionalized 1,2-dihydro-1-phosphet-2-one complex 23 through an unprecedented ring-expansion reaction; the products 21, 22, 23 were formed in a ratio of ca. 1:1:1. The structures of the 1H-phosphirene complex 9a, the 4-dimethylamino-substituted 2H-1,2-azaphosphole complex 10b, the bicyclic phosphirane complex 19, the phosphirane complex 21, and the 1,2-dihydro-1-phosphet-2-one complex 23 have been determined by single-crystal X-ray diffraction analysis.
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Synthesis and Spectroscopic Data of para-Substituted (3-Phenyl-2H-azaphosphirene)tungsten Complexes (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 257-261 
    Details
    ISSN: 1434-1948
    Keywords: Phosphorus heterocycles ; 2H-Azaphosphirene complexes ; Carbene complexes ; Tungsten ; Cyclizations ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-yield synthesis of para-substituted pentacarbonyl(3-phenyl-2H-azaphosphirene)tungsten complexes is reported, using a multi-step rearrangement reaction. Spectroscopic and mass-spectrometric data of these heterocyclic complexes are discussed; the 31P-NMR-chemical shifts clearly reflect the electronic influence of the para-phenyl substituents and the correlation with Hammett σp-constants is almost linear.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Phosphorus-Bridged Dinuclear Tungsten Amino(aryl)carbene Complexes - New Precursors for (2H-Azaphosphirene)tungsten Complexes bearing a σ-P-Bonded Cp* Group⋆ (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 2005-2012 
    Details
    ISSN: 1434-1948
    Keywords: Carbene complexes ; Tungsten ; Phosphorus ; 2H-Azaphosphirene complexes ; Cyclization ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first syntheses of pentacarbonyl[2-(pentamethyl-2,4-cyclopentadien-1-yl)-2H-azaphosphirene]tungsten complexes are reported, using a one-pot reaction of dichloro(pentamethyl-2,4-cyclopentadien-1-yl)phosphane (Cp*PCl2) with triethylamine and {[amino(aryl)carbene]pentcarbonyltungsten(0)}. [Pentamethyl-2,4-cyclopentadien-1-yl]phosphanediyl-bridged dinuclear carbene complexes are formed as long-lived intermediates, which, by elimination and rearrangement reactions, led to the final products. If traces of water were present, then by-products were formed; in one case, a dinuclear carbene complex with a P(Cp*)-O-P(Cp*) bridging unit was isolated. Under ordinary reaction conditions 2H-azaphosphirene complexes are slowly transformed into {pentacarbonyl[chloro(pentamethyl-2,4-cyclopentadien-1-yl)phosphane]tungsten(0)}. NMR-spectroscopic and single-crystal X-ray structural data of some dinuclear carbene complexes and 2-(pentamethyl-2,4-cyclopentadien-1-yl)-2H-azaphosphirene complexes are presented.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Polysulfonylamine. XLVI Molekülkomplexe von Di(organosulfonyl)aminen mit Dimethylsulfoxid und Triphenylphosphinoxid. Röntgenstrukturanalyse von Di(4-fluorbenzolsulfonyl)amin-Dimethylsulfoxid(2/1) (1993)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1945-1950 
    Details
    ISSN: 0044-2313
    Keywords: Di(organosulfonyl)amines ; addition compounds with dimethyl sulfoxide ; addition compounds with triphenylphosphine oxide ; preparation ; crystal and molecular structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. XLVI. Molecular Adducts of Di(organosulfonyl)amines with Dimethyl Sulfoxide and Triphenylphosphine Oxide. X-Ray Structure Determination of Di(4-fluorobenzenesulfonyl)amine-Dimethyl Sulfoxide(2/1)From equimolar solutions of the respective components in CH2Cl2/petroleum ether, the following crystalline addition compounds were obtained: (X—C6H4SO2)2NH … OS(CH3)2, where X = H, 4—CH3, 4—Cl, 4—Br, 4—I, 4—NO2 or 3—NO2; [(4—F—C6H4SO2)2NH]2 · (OS(CH)3)2 (8); (4—I—C6H4SO2)2NH · OP(C6H5)3. A (2/1) complex of (4—F—C6H4SO2)2NH with OP(C6H5)3 could not be isolated. The solid-state structure of the (2/1) compound 8 is compared with the known structure of the (1/1) complex (CH3SO2)2NH · OS(CH3)2. The crystallographic data for 8 at -95°C are: monoclinic, space group C2/c, a = 2 369.9(13), b = 1 006.8(4), c = 2 772.6(13) pm, β = 110.71(4)°, U = 6.187 nm3, Z = 8. Two N—H … O hydrogen bonds with N … O 275 and 280 pm connect the disulfonylamine molecules with the dimethyl sulfoxide molecule. The O atom of the latter has a trigonal-planar environment consisting of the S atom and the two hydrogen bond H atoms.
    Notes: Aus äquimolaren Lösungen der jeweiligen Komponenten in CH2Cl2/Petrolether wurden die folgenden kristallinen Addukte erhalten: (X—C6H4SO2)2NH · OS(CH3)2 mit X = H, 4—CH3, 4—Cl, 4—Br, 4—I, 4—NO2 und 3—NO2; [(4—F—C6H4SO2)2NH]2 · (OS(CH)3)2 (8); (4—I—C6H4SO2)2NH · OP(C6H5)3. Ein (2/1)-Komplex aus (4-F—C6H4SO2)2NH und OP(C6H5)3 ließ sich nicht isolieren. Die Festkörperstruktur des (2/1)-Addukts 8 wird mit der bekannten Struktur des (1/1)-Komplexes (CH3SO2)2NH · OS(CH3)2 verglichen. Kristallographische Daten von 8 bei -95°C: monoklin, Raumgruppe C2/c, a = 2 369,9(13), b = 1 006,8(4), c = 2 772,6(13) pm, β = 110,71(4)°, U = 6,187 nm3, Z = 8. Zwei Wasserstoffbrücken N—H … O mit N … O 275 bzw. 280 pm verknüpfen die Disulfonylamin-Moleküle mit dem Dimethylsulfoxid-Molekül. Das O-Atom des letzteren ist trigonal-planar vom S-Atom und den zwei Brücken-H-Atomen umgeben.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19936191120
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  • 6
    Electronic Resource
    Electronic Resource
    Polysulfonylamine. LXI [1]. Silber(I) in einer neuartigen N-Donor-Umgebung: Darstellung und Struktur von catena-Poly[(dimesylamido-N)(acetonitril)(μ-pyrazin)silber(I)] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 476-478 
    Details
    ISSN: 0044-2313
    Keywords: catena-Poly[(dimesylamido-N)(acetonitrile)(μ-pyrazine)] ; synthesis ; crystal and molecular structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. LXI. Silver(I) in a Novel N-Donor Environment: Synthesis and Structure of catena-Poly[(dimesylamido-N)(acetonitrile)(μ-pyrazine)silver(I)]The complex [Ag{N(SO2Me)2}(μ-pz)(MeCN)]∞ is precipitated upon adding pyrazine to an acetonitrile solution of AgN(SO2Me)2. Crystallographic data (at -100°C); monoclinic, space group P21/c, a = 912.3(2), b = 1 396.5(3), c = 1 151.7(3) pm, β = 97.20(2)°, U = 1.4557 nm3, Z = 4. The structure consists of infinite zigzag chains in the z-direction. The chain backbone is composed of silver atoms linked by pyrazine ligands (N—Ag—N 99.4°, Ag—N 232.4 und 234.0 pm). The severely distorted tetrahedral environment of Ag is completed by an N-bonded dimesylamide anion (Ag—N 224.3 pm) and an acetonitrile molecule (Ag—N 240.9 pm). The N—Ag—N angles vary from 97.5 bis 125.7°.
    Notes: Der Komplex [Ag{N(SO2Me)2}(μ-pz)(MeCN)]∞ wird durch Zugabe von Pyrazin zu einer Lösung von AgN(SO2Me)2 in Acetonitril ausgefällt. Kristallographische Daten (bei -100°C): monoklin, Raumgruppe P21/c, a = 912,3(2), b = 1 396,5(3), c = 1 151,7(3) pm, β = 97,20(2)°, U = 1,4557 nm3, Z = 4. Die Struktur besteht aus unendlichen Zickzack-Ketten in z-Richtung. Das Kettengerüst ist aus Silberatomen und verbrückenden Pyrazin-Liganden aufgebaut (N—Ag—N 99,4°, Ag—N 232,4 und 234,0 pm). Das Silber erreicht eine stark verzerrte tetraedrische Umgebung durch Koordination mit einem N-bindenden Dimesylamid-Anion (Ag—N 224,3 pm) und einem Acetonitril-Molekül (Ag—N 240,9 pm). Die N—Ag—N-Winkel variieren von 97,5 bis 125,7°.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210324
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  • 7
    Electronic Resource
    Electronic Resource
    Kristall- und Molekülstruktur von fac-Trichloro-tris(dimethylsulfoxid)bismut(III) BiCl3(DMSO)3 (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1037-1040 
    Details
    ISSN: 0044-2313
    Keywords: fac-Trichloro-tris(dimethyl sulfoxide)bismuth(III) ; crystal and molecular structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of fac-Trichloro-tris(dimethyl sulfoxide)bismuth(III) BiCl3(DMSO)3Crystals of the known, although structurally not characterized title compound were fortuitously obtained from a reaction mixture containing (CH3)3SiN(SO2CH3)2, BiCl3, DMSO, CH2Cl2 and CH3NO2. Crystallographic data (at -130°C): triclinic, space group P11, a = 816.1(5), b = 885.1(6), c = 1 360.6(8) pm, α = 77.58(3), β = 77.39(3), γ = 64.42(3)°, U = 0.8569 nm3, Z = 2. The DMSO ligands are bound through oxygen to the Bi atom. Important bond distances and angles in the resulting fac-octahedral complex are as follows: Bi—Cl 258.9, 261.0, 263.0, Bi—O 242.6, 245.7, 246.1 pm; Cl—Bi—O (trans) 170.3, 170.6, 176.9, Cl—Bi—Cl 94.6, 94.7, 96.0, O—Bi—O 81.7, 85.4, 87.9, Cl—Bi—O (cis) in the range 87.2-92.6, Bi—O—S 123.4, 126.1, 129.6°.
    Notes: Kristalle der bekannten, strukturell aber nicht untersuchten Titelverbindung entstanden zufällig in einer Reaktionsmischung aus (CH3)3SiN(SO2CH3)2, BiCl3, DMSO, CH2Cl2 und CH3NO2. Kristallographische Daten (bei -130°C): Triklin, Raumgruppe P1, a = 816,1(5), b = 885,1(6), c = 1 360,6(8) pm, α = 77,58(3), β = 77,39(3), γ = 64,42(3)°, U = 0,8569 nm3, Z = 2. Die DMSO-Liganden sind über Sauerstoff an das Bi-Atom gebunden. Die wichtigsten Bindungsabstände und -winkel des resultierenden fac-oktaedrischen Komplexes sind Bi—Cl 258,9, 261,0, 263,0, Bi—O 242,6, 245,7, 246,1 pm; Cl—Bi—O (trans) 170,3, 170,6, 176,9, Cl—Bi—Cl 94,6, 94,7, 96,0, O—Bi—O 81,7, 85,4, 87,9, Cl—Bi—O (cis) im Bereich 87,2-92,6, Bi—O—S 123,4, 126,1, 129,6°.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200615
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  • 8
    Electronic Resource
    Electronic Resource
    Drei stereoisomere quadratisch-pyramidale [Ma3b2]-Komplexe: Untersuchungen zur Existenz und zur Struktur kristalliner Dimethylsulfoxid-Komplexe von Antimon- und Bismuttrichlorid (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 229-238 
    Details
    ISSN: 0044-2313
    Keywords: Trichloro-bis(dimethyl sulfoxide)antimony(III)-antimony(III) chloride (1/1) ; trichloro-bis(dimethyl sulfoxide)antimony(III) ; trichloro-bis(dimethylsulfoxide)bismuth(III) ; trichloro-tris(dimethyl sulfoxide)bismuth(III) ; synthesis ; crystal and molecular structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Three Stereoisomeric Square-Pyramidal Complexes [Ma3b2]: Investigations of the Existence and the Structures of Crystalline Dimethyl Sulfoxide Complexes of Antimony and Bismuth TrichloridesThe formation of solid complexes MCl3 · n DMSO (M = Sb, Bi; n = 1-4) was reinvestigated. In each system, only two of four presumptive complexes could be isolated as crystalline solids: SbCl3 · DMSO (1 a) was prepared for the first time, SbCl3 · 2 DMSO (1 b), BiCl3 · 2 DMSO (2 b) and BiCl · 3 DMSO (2 c) were reproduced according to literature data. Evidence is presented as to the non-existence of BiCl3 · 4 DMSO, contrary to previous claims in the literature. A unit cell determination showed 2 c to be structurally identical with the monomeric fac-octahedral complex BiCl3(DMSO)3 obtained fortuitously and described elsewhere [Z. anorg. allg. Chem. 620 (1994) 1037]. The compounds 1 a (monoclinic, space group P21/c), 1 b (monoclinic, space group P21/n) and 2 b (monoclinic, space group C2) represent examples of each of the three possible geometric isomers of a square-pyramidal complex [Ma3b2]. In the formally 1/1 adduct 1 a, which is in fact [Sb(1)Cl3(DMSO)2 · Sb(2)Cl3], the Sb(1) atom of the complex unit displays square-pyramidal geometry with the DMSO ligands situated in the apical and one of the basal positions. These units are linked into chains by SbCl3 molecules acting as Cl-acceptors. Sb(2) forms two chelating chloro-bridges with cis-Cl atoms of one neighbouring complex and a third chloro-bridge with the remaining Cl of the symmetry-related second neighbour. The resulting Cl6-geometry around Sb(2) is distorted octahedral. 1 b consists of square-pyramidal molecules, in which the DMSO ligands occupy two basal cis-positions; the monomeric units are loosely linked through the apical Cl atoms to form a chain of octahedra sharing trans-vertices. The asymmetric unit of 2b is a square pyramid with trans-basal DMSO ligands. The pyramids are connected by symmetry-equivalent basal chlorine atoms into chains of octahedra sharing cis-vertices. 1a displays remarkably short Sb—O dative bonds (204.7/212.9 pm); the M—O bond distances of 1b and 2b are 223.0/234.6 and 234.5/238.7 pm, respectively.
    Notes: Die Bildung kristalliner Komplexe MCl3 · n DMSO (M = Sb, Bi; n = 1-4) wurde erneut untersucht. In beiden Systemen konnten nur je zwei der vier vermuteten Komplexe als kristalline Feststoffe isoliert werden, und zwar SbCl3 · DMSO (1 a) erstmalig, die Addukte SbCl3 · 2 DMSO (1 b), BiCl3 · 2 DMSO (2 b) und BiCl3 · 3 DMSO (2 c) durch Nacharbeiten von Literaturvorschriften. Der in der Literatur beschriebene Komplex BiCl3 · 4 DMSO existiert offenbar nicht. Die Bestimmung der Elementarzelle ergab für 2 c strukturelle Identität mit dem zufällig erzeugten fac-oktaedrischen BiCl3(DMSO)3 [Z. anorg. allg. Chem. 620 (1994) 1037]. Die Verbindungen 1 a monoklin, Raumgruppe P21(c), 1 b (monoklin, Raumgruppe P21/n) und 2 b (monoklin, Raumgruppe C2) sind Beispiele für die drei möglichen geometrischen Isomere eines quadratisch-pyramidalen [Ma3b2]-Komplexes. Das formale 1/1-Addukt 1 a ist ein Zweikernkomplex [Sb(1)Cl3(DMSO)2 · Sb(2)Cl3], dessen Sb(1)-Atom quadratisch-pyramidal mit den DMSO-Liganden in der apikalen und einer basalen Position koordiniert ist. Diese Einheiten sind über SbCl3-Moleküle, die dals Cl-Akzeptoren wirken, zu Ketten verknüpft. Sb(2) bildet zwei chelatartige Chlorobrücken mit cis-Chloratomen der einen komplexen Nachbareinheit und eine dritte Chlorobrücke mit dem verbleibenden Chloratom des symmetrieäquivalenten anderen Nachbarkomplexes. Die resultierende Cl6-Geometrie um Sb(2) ist verzerrt oktaedrisch. In den quadratisch-pyramidalen Molekülen von 1 b besetzen die DMSO-Liganden zwei basale cis-Positionen; die monomeren Einheiten sind locker über das apikale Chlor zu Ketten aus trans-eckenverknüpften Oktaedern assoziiert. Die asymmetrische Einheit von 2 b ist eine quadratische Pyramide mit trans-basalen DMSO-Liganden; die Pyramiden sind über symmetrieäquivalente basale Chloratome zu Ketten aus cis-eckenverknüpften Oktaedern verbunden. Die dativen Sb—O-Bindungen in 1 a sind mit 204,7/212,9 pm bemerkenswert kurz; die M—O-Abstände in 1 b und 2 b betragen 223,0/234,6 bzw. 234,5/238,7 pm.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210212
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