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Organische Synthesen mit übergangsmetall-Komplexen, 51. 1-Metalla-1,3,5-triene und 1-Metalla-1,3-dien-5-ine von Chrom und Wolfram durch Insertion von Alkinen in M=C- bzw. C=C-Bindungen von 1-Metalla-1,3-dienen bzw. 1-Metalla-1-en-2-inen (1991)

Aumann, Rudolf ; Heinen, Heinrich ; Hinterding, Peter ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 1229-1236

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ISSN: 0009-2940

Keywords: Carbene complexes of chromium and tungsten ; 1-Metalla-1,3,5-trienes ; 1-Metalla-1,3-dien-5-ynes ; Insertion of alkynes into M=C and C=C bonds ; [2 + 2] Cycloaddition reactions of carbene complexes and alkynes ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Organic Syntheses via Transition Metal Complexes, 51. - 1-Metalla-1,3,5-trienes and 1-Metalla-1,3-dien-5-ynes of Chromium and Tungsten by Insertion of Alkynes into M=C and C=C Bonds of 1-Metalla-1,3-dienes and 1-Metalla-1-en-3-ynes, respectively1-Metalla-1,3,5-trienes LnM=C(NEt2)-C(Me)—C(OEt)-CH=CHPh (3,4) and LnM=C(OEt)- CH=C(NEt2) - C(Me)=CHPh [5, LnM=Cr(CO)5 (a), W(CO)5 (b)] are obtained for the first time from the corresponding 1-metalla-1,3-dienes LnM=C(OEt) - CH=CHPh (1a, b) under very mild conditions by the insertion of the electron-rich alkyne Et2N-C ≡ C - Me (2) into the M=C and the C=C bonds, respectively, of 1. The chelate complex (6b) and the cyclobutenyl carbene complex 7b are isolated as minor side products. 1-Metalla-1,3-dien-5-ynes LnM=C(NEt2) - C(Me)=C(OEt) - C ≡ CPh [9, 10, LnM=Cr(CO)5 (a), W(CO)5 (b)] are formed with high regio- and stereoselectivity on insertion of 2 into the M=C bonds of 1-metalla-1-en-3-ynes 8. X-ray data are given for the tungsten complex 3b.

Additional Material: 1 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/cber.19911240541

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Reaktive E = C(p - p)π-Systeme, XXXI Erste Vertreter aminosubstituierter 1,2,4-Diazaphosphole (1992)

Grobe, Joseph ; Van, Due Le ; Hegemann, Marianne ; [et al.]

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 411-414

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ISSN: 0009-2940

Keywords: Phosphaalkyne, amino- ; [3 + 2] Cycloaddition ; 1,2,4-Diazaphospholes ; 1,2,3-Diazaphospholes ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Notes: Reactive E = C(p - p)π Systems, XXXII[1]. - First Representatives of Amino-Substituted 1,2,4-Diazaphospholes(Diisopropylamino)phosphaethyne iPr2N - C≡P reacts at 20° C in a [3 + 2] cycloaddition with (trifluoromethyl)diazomethane (2a) or methyl diazoacetate (2b) to yield a mixture of the corresponding regioisomers 1H-1,2,4-diazaphospholes (5a or 5b) and 1H-1,2,3-diazaphospholes (6a or 6b) in quantitative yields (isomer ratio: 5a/6a = 2:1; 5b/6b = 4:1). X-ray diffraction studies on 5a and 5b indicate a delicate charge balance in the bonding system of 1H-1,2,4,σ2-diazaphospholes under the influence of the exocyclic push/pull substituents iPr2N and CF3 or CO2Me, respectively.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/cber.19921250219

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Reaktive E = C(p-p)π-Systeme. XLII [1]. Neue Koordinationsverbindungen des 2-(Diisopropylamino)-1-phosphaethins: [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}], [(Ph3P)2Pt{η2-(iPr2NCP)}] und [Co2(CO)6{η2-η2-(iPr2NCP)}]In memoriam Wilhelm Klemm (1996)

Grobe, Joseph ; Le Van, Duc ; Immel, Franz ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 622 (1996), S. 24-34

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ISSN: 0044-2313

Keywords: Phosphaalkyne, amino- ; nickel, platinum, cobalt complexes ; 1 λ3, 3 λ5-diphosphetene ; 1H, 13C{1H} and 31P{1H} NMR spectra ; X-ray structure determination ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Reactive E = C(pp)π-Systems. XLII [1]. Novel Coordination Compounds of 2-(Diisopropylamino)-1-phosphaethyne: [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}], [(Ph3P)2Pt{η2-(iPr2NCP)}], and [Co2(CO)6{η2-μ2-(iPr2NCP)}]2-(Diisopropylamino)-phosphaethyne iPr2N—C≡P (2) reacts with the Ni(0)-complexes [Ni(1,5-cyclooctadiene)2] and [Ni(CO)3(1-azabicyclo[2.2.2]octane)], respectively, to give the novel complex [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}] (5), with the 1,3-diphosphacyclobutadiene derivative and 2 (side-on) as π-ligands. The molecular structure of 5 determined by X-ray diffraction on single crystals proves the spin systems and rotational barriers deduced from NMR-data (1H, 13C-, 31P). The PC distances of the four-membered ring of 1.817(2) and 1.818(2) Å - as expected - are considerably longer than the PC bond of the η2-coordinated phosphaalkyne 2 [1.671(2) Å]. - In the reactions of 2 with [(Ph3P)2Pt(C2H4)] or [Co2(CO)8] the ligand properties of 2 resemble those of alkynes affording the complexes [(Ph3P)2Pt{η2-(iPr2NCP)}] (7) with side-on coordinated 2 and [Co2(CO)6{η2-μ2-(iPr2NCP)}] with 2 acting as a 4e donor bridge in quantitative yield.In attempts to prepare copper(I) complexes of the aminophosphaalkyne 2 by reaction with CuCl or CuI the only isolable product formed in reasonable amounts under the influence of air and moisture is the 1 λ3, 3 λ5-diphosphetene (iPr2N) (10) (isolated yield: ca. 20%). The crystal structure analysis of 10 indicates a strong structural relationship to the diamino-2-phosphaallyl cation [Me(iPr2N)]+ (12), the 1,3-diphosphacyclobutadiene ligand (iPr2NCP)2 in the binuclear complex [{η1, μ2-(iPr2NCP)2}Ni2(CO)6] (3a) as well as to the heterocycles (dme)2LiOE2′ (E′ = S, 11a; E′ = Se, 11b) prepared by Becker et al. [11b, 35].

Notes: 2-(Diisopropylamino)-phosphaethin iPr2N-C≡P (2) reagiert mit den Ni(0)-Komplexen [Ni(1,5-Cyclooctadien)2] bzw. [Ni(CO)3(1-Azabicyclo[2.2.2]octan)] zu dem neuen Komplex [{η4-(iPr2NCP)2}Ni{η2-(iPr2NCP)}] (5), der zwei Moleküle 2 in Form des 1,3-Diphosphacyclobutadiensystems und ein Molekül 2 „side-on“ koordiniert als π-Liganden enthält. Die Molekülstruktur von 5, ermittelt durch Röntgenbeugung an Einkristallen, bestätigt die aus den NMR-Daten (1H-, 13C-, 31P) abgeleiteten Spinsysteme und Rotationsbarrieren. Die PC-Abstände des Vierrings sind mit 1,817(2) bzw. 1,818(2) Å erwartungsgemäß erheblich länger als die PC-Bindung des η2-koordinierten Phosphaalkins 2 [1,671(2) Å]. Bei den Umsetzungen von 2 mit [(Ph3P)2Pt(C2H4)] bzw. [Co2(CO)8] entspricht das koordinative Verhalten dem von Alkinen; sie liefern die Komplexe [(Ph3P)2Pt{η2-(iPr2NCP)}] (7) mit side-on gebundenem 2 bzw. [Co2(CO)6{η2-η2-(iPr2NCP)}] mit 2 als 4e-Donorbrücke in quantitativer Ausbeute.Bei dem Versuch, aus 2 und CuCl bzw. CuI Kupfer(I)-Komplexe des Aminophosphaalkins darzustellen, bildet sich unter Einwirkung von Luft und Feuchtigkeit als einziges isolierbares Produkt das 1λ3, 3λ5-Diphospheten (iPr2N) (10) in beträchtlicher Menge (Reinausbeute: ca. 20%). Für 10 ergibt sich aus der Kristallstrukturanalyse eine enge Beziehung zu dem Diamino-2-phosphaallyl-Kation [Me(iPr2N)]+ (12), dem 1,3-Diphosphacyclobutadien-Liganden (iPr2NCP)2 im Zweikernkomplex [{η1-μ2-(iPr2NCP)2}Ni2(CO)6] (3a) sowie zu den von Becker et al. [11 b, 35] dargestellten Heterocyclen (dme)2LiOE2′ (E′ = S, 11a; E′ = Se, 11b).

Additional Material: 6 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19966220106

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Synthese, Struktur und Eigenschaften der neuen trinuklearen Halogenoselenate(IV) [Se3Cl13]- und [Se3Br13]- Kristallstrukturen von [Ph3C][Se3Cl13] und [Ph3C][Se3Br13]Frau Professor Marianne Baudler zum 70. Geburtstage am 27. April 1991 gewidmet (1991)

Ahlers, Frank-Peter ; Lührs, Erhard ; Krebs, Bernt

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 594 (1991), S. 7-22

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ISSN: 0044-2313

Keywords: Trimeric haloselenates(IV) ; syntheses ; crystal structures ; i.r., Raman spectra ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Synthesis, Structure, and Properties of the Novel Trinuclear Haloselenates(IV) [Se3Cl13]- and [Se3Br13]-. Crystal Structures of [Ph3C][Se3Cl13] and [Ph3C][Se3Br13]As the first intermediates in the stepwise degradation of the cubanelike tetrameric selenium(IV) halides [SeCl4]4 and [SeBr4]4 in organic solvents the trimeric haloselenate(IV) anions [Se3Cl13]- could be isolated. From acetonitrile as solvent it was possible to obtain red-brown [Ph3C][Se3Cl13] (1) (space group P1, a = 10.199(4), b = 10.426(3), c = 15.451(5) Å, α = 96.97(3), β = 91.65(3), γ = 107.48(2)° at 140 K). Dark-red [Ph3C][Se3Br13] (2) (space group P21/c, a = 11.258(6), b = 16.367(9), c = 26.280(11) Å, β = 114.70(4)° at 140 K) was stabilized as the corresponding bromoselenate(IV) from a dichloromethane solution. The isostructural anions of 1 and 2 consist of three octahedral SeX6 units, which are connected via cis-edges to form a trimeric anion, so that a μ3-halogen atom results. The mean bond distances are for terminal Se—X bonds 2.197 Å (Cl) resp. 2.391 Å (Br), for Se-μ2X 2,601 Å (Cl) resp. 2.782 Å (Br) and for Se-μ3X 2.782 Å (Cl) resp. 2.904 Å (Br). Infrared and Raman spectra of [Se3Cl13]- and [Se3Br13]- are reported.

Notes: Mit den trimeren Halogenoselenat(IV)-Anionen [Se3Cl13]- und [Se3Br13]- gelang es, die ersten Zwischenstufen des sukzessiven Abbaus der cuban-artigen tetrameren Selentetrahalogenide [SeCl4]4 und [SeBr4]4 in organischen Lösungsmitteln zu isolieren und röntgenstruktur-analytisch zu charakterisieren. Aus Acetonitril als Lösungsmittel konnte das rotbraune [Ph3C][Se3Cl13] (1) (Raumgruppe P1, a = 10,199(4), b = 10,426(3), c = 15,451(5) Å, α = 96,97(3), β = 91,65(3), γ = 107,48(2)° bei 140 K) dargestellt werden. In dem dunkelroten [Ph3C][Se3Br13] (2) (Raumgruppe P21/c, a = 11,258(6), b = 16,367(9), c = 20,280(11) Å, β = 114,70(4)° bei 140K) wurde aus Methylenchlorid das entsprechende Bromoselenat(IV) isoliert. Die beiden isostrukturellen Anionen von 1 und 2 sind jeweils aus drei oktaedrischen SeX6-Einheiten aufgebaut, die über gemeinsame cis-ständige Kanten zu einem trimeren Anion verknüpft sind, so daß ein μ3-verbrückendes zentrales Halogenatom entsteht (X = Cl, Br). Die mittleren Bindungslängen betragen für die terminalen Se—X-Bindungen 2,197 Å (Cl) bzw. 2,391 Å (Br), für Se-μ2X 2,601 Å (Cl) bzw. 2,782 Å (Br) und für Se-μ3X 2,782 Å (Cl) bzw. 2,904 Å (Br). Über schwingungsspektroskopische Untersuchungen wird berichtet.

Additional Material: 5 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19915940102

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Thallium(I)-Thiolate: Darstellung, Struktur und Eigenschaften von TlSC6H5, TlS-t-C4H9 und TlSC7H7Professor Kurt Dehnicke zum 60. Geburtstage gewidmet (1991)

Krebs, Bernt ; Brömmelhaus, Andreas

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 595 (1991), S. 167-182

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ISSN: 0044-2313

Keywords: Thallium(I) thiolates ; syntheses ; crystal structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Thallium(I) Thiolates: Synthesis, Structure, and Properties of TlSC6H5, TlS-t-C4H9, and TlSC7H7By reaction of thallium(I) salts with sodium thiolates in organic solvents it is possible to synthesize and crystallize polymeric and oligomeric neutral thallium(I) thiolate complexes. The polymeric crystal structure of yellow benzenethiolato thallium(I) TlSC6H5 (space group P213, a = 19.943(3) Å at 143 K) is built up by the two novel structure units [Tl7(SC6H5)6]+ and [Tl5(SC6H5)6]-. Yellow tert.-butanethiolato thallium(I) TlS-t-C4H9 (space group P1, a = 11.490(3), b = 11.490(3), c = 12.698(4) Å, α = 108.31(3), β = 91.21(2), σ = 116.99(3)° at 143 K) consists of [Tl8(S-t-C4H9)8] molecules, the thallium atoms being either in trigonal pyramidal or ψ-trigonal bipyramidal coordination. Yellow phenylmethanethiolato thallium(I) TlSC7H7 crystallizes as thin plates (space group: Pbcn, a = 31.215(9), b = 7.173(2), c = 7.184(2) Å at 293 K). The crystal structure contains chains of fourmembered Tl2S2 rings which are linked through trans edges to form a ladder-like arrangement. Each thallium atom is coordinated trigonal-pyramidally by three sulfur atoms. The vibrational spectra of the compounds are reported.

Notes: Durch Umsetzung von Thallium(I)-Salzen mit Natriumthiolaten in organischen Lösungsmitteln gelang die Synthese und Kristallisation von polymeren und oligomeren neutralen TlI-Thiolat-Komplexen. Das gelbe Benzolthiolatothallium(I) TlSC6H5 (Raumgruppe P213, a = 19,943(3) Å bei 143 K) enthält in der polymeren Kristallstruktur die zwei neuartigen Strukturelemente [Tl7(SC6H5)6]+ und [Tl5(SC6H5)6]-. Die Thallium-Atome sind entweder trigonal-pyramidal oder ψ-trigonal-bipyramidal koordiniert. Das gelbe tert.-Butanthiolato-thallium(I) TlS-t-C4H9 (Raumgruppe P1, a = 11,490(3), b = 11,490(3), c = 12,698(4) Å, α = 108,31(3), β = 91,21(2), σ = 116,99(3)° bei 143 K) wird aus [Tl8(S-t-C4H9)8]-Molekülen aufgebaut, wobei die Thallium-Atome wieder trigonal-pyramidal und ψ-trigonal-bipyramidal koordiniert sind. Phenylmethanthiolato-thallium(I) TlSC7H7 kristallisiert in Form dünner gelber Plättchen (Raumgruppe: Pbcn, a = 31,215(9), b = 7,173(2), c = 7,184(2) Å bei 293 K). Die Kristallstruktur enthält Thallium-Thiolat-Ketten, die strickleiterartig aus trans-verknüpften Tl2S2-Vierringen bestehen. Jedes Thallium-Atom ist trigonal-pyramidal von drei Schwefel-Atomen koordiniert. Über schwingungsspektroskopische Untersuchungen wird berichtet.

Additional Material: 7 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19915950116

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