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  • synthesis  (8)
  • crystal and molecular structure  (4)
  • Cyclizations  (3)
  • 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.
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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 
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    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.
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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.
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  • 4
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    Electronic Resource
    Polysulfonylamine. LXXIII [1]. Metall(II)-dimesylamid-Tetrahydrate: Das Dimesylamid-Anion als einzähniger O-Ligand und tetrafunktioneller Wasserstoffbrücken-Akzeptor in den isotypen Komplexen [M(H2O)4 {(CH3SO2)2N}2] mit M = Magnesium, Nickel, Kupfer und Zink (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1065-1075 
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    ISSN: 0044-2313
    Keywords: Bis(dimesylamido-O)tetraaquametal(II) complexes ; synthesis ; X-ray structures ; isotypic series ; Jahn-Teller distortion ; hydrogen bond pattern ; graph-theoretical analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonyl Amines. LXXIII. Metal(II) Dimesylamide Tetrahydrates: The Dimesylamide Anion as a Monodentate O-Ligand and a Tetrafunctional Hydrogen Bond Acceptor in the Isotypic Complexes [M(H2O)4{(CH3SO2)2N}2], where M = Magnesium, Nickel, Copper, or ZincBy treating aqueous HN(SO2CH3)2 solutions with the appropriate metal hydroxides, oxides, or carbonates, the crystalline tetrahydrates M[(CH3SO2)2N]2 · 4 H2O (M = Mg, Ca, Mn, Co, Ni, Cu, Zn, Cd) were obtained and analytically characterized. The crystal structures of the Mg, Ni, Cu and Zn compounds, as determined by single-crystal X-ray diffraction at low temperatures, reveal an isotypic series (triclinic, space group P1, Z = 1). The structures consist of centrosymmetric trans-octahedral [M(H2O)4{(CH3SO2)2N}2] molecules in which the anionic ligand acts as a monodentate O-donor. For the Mg, Ni and Zn complexes, the M—OH2 and M—O(anion) distances lie in the ranges 203-206 pm and 209-214 pm, respectively. The copper compound features a marked Jahn-Teller distortion with Cu—OH2 = 195.8 and 197.7 pm and Cu—O(anion) = 232.5 pm. The cis-angles O—M—O of the four molecules do not deviate appreciably from 90°. The complex units are associated through a highly organized three-dimensional hydrogen bond network in which all the water protons act as donors and the non-coordinating oxygen atoms and the nitrogen atom of the anionic ligand are involved as acceptors. The H-bond pattern is subjected to a graph-theoretical analysis at the first and second levels.
    Notes: Die kristallinen Tetrahydrate M[(CH3SO2)2N] · 4 H2O (M = Mg, Ca, Mn, Co, Ni, Cu, Zn, Cd) wurden durch Neutralisation wäßriger HN(SO2CH3)2-Lösungen mit entsprechenden Metallhydroxiden, -oxiden oder -carbonaten erhalten und analytisch charakterisiert. Nach Aussage von Tieftemperatur-Röntgenstrukturbestimmungen bilden die Verbindungen mit M = Mg, Ni, Cu und Zn eine isotype Reihe (triklin, Raumgruppe P1, Z = 1). Die Strukturen bestehen aus trans-oktaedrischen und inversionssymmetrischen [M(H2O)4{(CH3SO2)2N}2]-Molekülen mit einzähnig O-bindenden anionischen Liganden. Für die Komplexe mit M = Mg, Ni und Zn werden M—OH2- und M—O(Anion)-Bindungslängen im Bereich 203-206 beziehungsweise 209-214 pm beobachtet. Die Kupferverbindung zeigt eine deutliche Jahn-Teller-Verzerrung mit Cu—OH2 = 195,8 und 197,7 pm und Cu—O(Anion) = 232,5 pm. In keinem der vier Moleküle weichen die cis-Winkel O—M—O stark von 90° ab. Die Komplexeinheiten sind über ein hochgradig organisiertes dreidimensionales Wasserstoffbrücken-Netz miteinander verknüpft, in welchem sämtliche Wasserprotonen als Donoren fungieren und die nichtkoordinierenden Sauerstoffatome des anionischen Liganden ebenso wie dessen Stickstoffatom als Akzeptoren wirken. Das H-Brücken-Muster wird einer graphentheoretischen Analyse auf erstem und zweitem Niveau unterzogen.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220622
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  • 5
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    Polysulfonylamine. LXXXIV [1]. Zur Isotypie in den Dimesylamid-Komplexreihen [M(H2O)4{(CH3SO2)2N}2] (M=Mg, Ca, Ni, Cu, Zn, Cd) und [M(py)4{(CH3SO2)2N}2] (M=Ni, Cu, Zn, Cd) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1175-1182 
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    ISSN: 0044-2313
    Keywords: Bis(dimesy1amido-O)tetraaquametal(II) complexes ; bis(dimesy1amido-O)tetrapyridinemetal(II) complexes ; synthesis ; X-ray structure; isotypic series ; Jahn-Teller distortion ; O—H…O, O—H…N and C—H…O hydrogen bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonylamines. LXXXIV. Isotypic Structures in the Dimesylamide Complex Series [M(H2O)4{(CH3SO2)2N}2] (M=Mg, Ca, Ni, Cu, Zn, Cd) and [M(py)4{(CH3SO2)2N}2] (M=Ni, Cu, Zn, Cd)The crystal structures of the trans-octahedral complexes [M(H2O)4{(CH3SO2)2N}2] (M=Ca, Cd), in which the dimesylamide anion acts as a monodentate O-ligand and a tetrafunctional hydrogen bond acceptor, were determined by low-temperature X-ray diffraction. Both belong to an isotypic series (triclinic, space group P1, Z = 1) that had previously been characterized for M=Mg, Ni, Cu and Zn (Z. Anorg. Allg. Chem. 1996, 622, 1065). In this structure there exists an extended network of strong hydrogen bonds which is probably the underlying reason why the structure type surprisingly persists across the whole series. To support this explanation by indirect evidence from comparison with suitable structures devoid of strong hydrogen bonding, the analogous trans-octahedral complexes [M(py)4{(CH3SO2)2N}2] (M=Mn, Co, Ni, Cu, Zn, Cd) were prepared by treating M[(CH3SO2)2N]2 with pyridine, and the crystal structures of the Ni, Cu, Zn and Cd compounds were studied by low-temperature X-ray crystallography. As anticipated, the four pyridine complexes do not form an isotypic series but instead two isotypic pairs consisting of the Ni and Zn compounds (monoclinic, space group P21/n, Z =2) and of the Cu and Cd complexes (triclinic, space group P1, Z = 1). All molecules of the aqua and the pyridine complexes display crystallographic centrosymmetry. In the hydrates, the mean M—OH2 and the M—O(anion) distances are 232.6 and 232.7 pm for M = Ca, 225.5 and 230.3 pm für M = Cd. The mean M—N and the M—O(anion) bond lengths of the pyridine species amount to 211.8 and 213.1 pm for M = Ni, 217.0 and 218.5 pm for M = Zn, 232.8 and 234.4 pm for M = Cd; the corresponding values for the severely Jahn-Teller distorted Cu complex are 203.6 and 254.5 pm. In the crystals of the pyridine complexes, each methyl group is connected through a weak C—H…O bond to a sulfonyl oxygen atom of an adjacent molecule.
    Notes: Die Kristallstrukturen der trans-oktaedrischen Komplexe [M(H2O)4{(CH3SO2)2N}2] (M=Ca, Cd), in denen das Dimesylamid-Anion als einzähniger O-Ligand und tetrafunktioneller Wasserstoffbrücken-Akzeptor wirkt, wurden durch Tieftemperatur-Röntgenbeugung ermittelt. Beide gehören zu einer isotypen Reihe (triklin, Raumgruppe P1, Z = 1), die zuvor für M=Mg, Ni, Cu und Zn charakterisiert worden war (Z. Anorg. Allg. Chem. 1996, 622, 1065). Hauptursache für die überraschende Persistenz der Isotypie in der gesamten Reihe ist vermutlich das in der Struktur auftretende hochorganisierte Netzwerk aus starken intermolekularen Wasserstoffbrücken. Um diese Annahme durch indirekte Evidenz an vergleichbaren Strukturen ohne starke H-Brücken zu überprüfen, wurden die analogen trans-oktaedrischen Komplexe [M(py)4{(CH3SO2)2N}2] (M=Mn, Co, Ni, Cu, Zn, Cd) aus M[(CH3SO2)2N]2 und Pyridin dargestellt und die Vertreter mit M=Ni, Cu, Zn und Cd durch Tieftemperatur-Röntgenbeugung untersucht. Der Erwartung entsprechend bilden die vier Pyridin-Komplexe keine isotype Reihe, aber zwei isotype Paare, die aus der Ni- und der Zn- Verbindung (monoklin, Raumgruppe P21/n, Z = 2) bzw, dem Cu- und dem Cd-Komplex (triklin, Raumgruppe P1, Z = 1) bestehen. Sämtliche Moleküle besitzen kristallographische Inversionssymmetrie. Die Mittelwerte der M—OH2- und die M—O(Anion)-Abstände in den Wasser-Komplexen betragen 232,6 und 232,7 pm für M=Ca, 225,5 und 230,3 pm für M=Cd. In den Pyridin-Komplexen sind die mittleren M—N- und die M—O(Anion)-Bindungslängen 211,8 und 213,1 pm für M=Ni, 217,0 und 218,5 pm für M=Zn, 232,8 und 234,4 pm für M=Cd sowie 203,6 und 254,5 pm für den eine erhebliche Jahn-Teller-Verzerrung aufweisenden Cu-Komplex. In den Kristallen der Pyridin-Komplexe ist jede Methylgruppe über eine schwache C—H … O-Wechselwirkung mit einem Sulfonyl-Sauerstoffatom eines Nachbarmoleküls verknüpft.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230728
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  • 6
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    Electronic Resource
    Polysulfonylamine. LXXVII. Synthese neuer Triorganoelement(IV)-di(fluorsulfonyl)amide R3EN(SO2F)2 (E = Si, Ge, Sn, Pb) und Kristallstrukturen von Me3PbN(SO2F)2 und CsN(SO2F)2 (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 324-332 
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    ISSN: 0044-2313
    Keywords: Triorganoelement(IV) di(fluorosulfonyl)amides ; main group 4 elements ; cesium di(fluorosulfonyl)amide ; synthesis ; x-ray structures ; C-H … O hydrogen bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polysulfonylamine. LXXVII. Synthesis of new Triorganoelement(IV) Di(fluorosulfonyl)amides R3EN(SO2F)2 (E = Si, Ge, Sn, Pb) and Crystal Structures of Me3PbN(SO2F)2 and CsN(SO2F)2The following compounds were prepared for the first time and/or by new procedures [Z = N(SO2F)2]: Me3SiZ (1 b), Ph3SnZ (3f), Me3PbZ (4a) and Ph3PbZ (4 b) by metathesis of the corresponding R3ECI with AgZ or AgZ·C6H6; Me3GeZ(2),Me3SnZ, 4 a and 4b by acidolysis of R4E with HZ; cHex3SnZ (3e) by neutralization of cHex3SnOH with HZ. Compounds 1b, 2, 3e, 3f, 4a and 4b have not been reported previously. The crystal structures of 4a (triclinic, space group P1) and of Cs⊕Z⊖ (8; monoclinic, space group P21/n) were determined by low-temperature X-ray diffraction. The asymmetric unit of 4 a consists of an ion pair Me3Pb⊕Z⊖, connected by a lead-nitrogen bond and a weak lead-oxygen interaction (Pb—N 260.3, Pb …O 337.5 pm). The pairs are linked by a lead-oxygen interaction (Pb—O′ 261,5 pm) to form parallel chains and further by five independent C—H…O hydrogen bonds (H…O 250-275 pm) to form a three-dimensional network. In the crystal of 8, the anion is surrounded by seven cations, displaying eleven Cs—X bonding interactions (1 × Cs—N 321.1 pm, 6 × Cs—O in the range 308.5—323.6 pm, 2 × Cs—F 337.3 and 338.0 pm, 1 × Cs—F 369.5 pm and 1 × Cs—O 375.3 pm). The irregular coordination polyhedron of the cation is best described by a coordination number of 9 + 2. The conformation of Z⊖ in both structures does not deviate appreciably from the pseudo C2-symmetry that is observed for the same anion in onium salts.
    Notes: Die folgenden Verbindungen wurden erstmalig und/oder nach neuen Verfahren synthetisiert [Z = N(SO2F)2]: Me3SiZ durch Transaminierung von HZ mit (Me3Si)2NH; Ph3SiZ (1b), Ph3SnZ (3f), Me3PbZ (4a) und Ph3PbZ (4b) durch Metathese des entsprechenden R3EC1 mit AgZ oder AgZ · C6H6; Me3GeZ (2), Me3SnZ, 4 a und 4b durch Acidolyse von R4E mit HZ; cHex3SnZ (3e) durch Neutralisation von cHex3SnOH mil HZ, Bel 1b, 2, 3e, 3f, 4a und 4b handelt es sich um neue Verbindungen. Die Kristallstrukturen von 4a (triklin, Raumgruppe P1) und von Cs⊕Z⊖ (8; monoklin, Raumgruppe P21/n) wurden durch Tieftemperatur-Röntgenbeugung ermittelt. Die asymmetrische Einheit von 4a besteht aus einem Ionenpaar Me3Pb⊕Z⊖, das durch eine Blei-Stickstoff-Bindung und eine schwache Blei-Sauerstoff-Wechselwirkung gebildet wird (Pb—N 260,3, Pb … O 337,5 pm). Die Ionenpaare sind über eine Blei-Sauerstoff-Wechselwirkung (Pb—O′ 261,5 pm) zu parallelen Ketten assoziiert, die ihrerseits über fünf unabhängige C—H … O-Wasserstoffbrücken (H … O 250-275 pm) ein dreidimensionales Netz aufbauen. Im Kristall von 8 ist das Anion von sieben Kationen umgeben, wobei insgesamt elf als bindend einzustufende Cs—X-Wechselwirkungen auftreten (1× Cs—N 321,1 pm, 6× Cs—O im Bereich 308,5 323,6 pm, 2 × Cs—F 337,3 und 338,0 pm, 1 × Cs—F 369,5 pm und 1 × Cs—O 375,3 pm). Das unregelmäßige Koordinationspolyeder des Kations wird am besten mit der Koordinationszahl 9 + 2 beschrieben. In beiden Strukturen weicht die Konformation des Anions nicht wesentlich von der Pseudo-C2-Symmetrie des diskreten Z⊖ in bekannten Onium-Salz-Strukturen ab.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19976230152
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  • 7
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    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 
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    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.
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    URL: http://dx.doi.org/10.1002/zaac.19936191120
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  • 8
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    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 
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    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°.
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    URL: http://dx.doi.org/10.1002/zaac.19956210324
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  • 9
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    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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    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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