Cyclothiazeno-Komplexe des Wolframs mit Phosphaniminatound tertiär-Butoxyliganden

1999

Z. anorg. allg. Chem.

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Die Metalla‐Cyclothiazeno‐Komplexe (Cyclo‐1λ6‐metalla‐3,5‐dithia‐2,4,6‐triazino‐Komplexe) [{Mo(N3S2)(Cl) · (OtBu)2}{Mo(O)(N3S2)(OtBu)}]2 (1) und [W(N3S2)2(LiCl) · {N≡W(NPPh3)3}2] (2) entstehen aus [MoCl3(N3S2)]2 und LiOtBu in Toluol, bzw. aus [WCl3(N3S2)]2 und LiNPPh3 in THF. Beide Komplexe bilden feuchtigkeitsempfindliche, schwarze (1) bzw. braune (2) Kristalle, die wir durch Kristallstrukturanalysen charakterisiert haben. 1 · Toluol: Raumgruppe P 1, Z = 1, Gitterabmessungen bei –83 °C: a = 934,2(1); b = 964,4(1); c = 1700,3(1) pm; α = 83,54(1)°; β = 78,35(1)°; γ = 71,56(1)°, R1 = 0,0339. 2 · 1,625 Toluol · 0,75 THF: Raumgruppe P 1, Z = 4, Gitterabmessungen bei –80 °C: a = 1313,8(1); b = 2896,8(2); c = 3384,9(3) pm; α = 82,42(1)°; β = 88,71(1)°; γ = 77,28(1)°, R1 = 0,0603.

“…Typ C AsPh 4 [W 2 Cl 4 2 Cl 2 (N 3 S 2 )] [9] [WCl 2 (N 3 S 2 )(NPPh 3 )(Pyridin)] [13] [WCl 2 (N 3 S 2 )(NPMe 3 )(Pyridin)] [13] Typ…”

Section: New Coordination Motives At Cyclothiazeno Complexes Of Molybmentioning

confidence: 99%

Section: [W(n 3 S 2 ) 2 (Licl){nºw(npph 3 ) 3 } 2 ] (2)unclassified

Section: [W(n 3 S 2 ) 2 (Licl){nºw(npph 3 ) 3 } 2 ] (2)mentioning

confidence: 99%

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Neue Koordinations-Motive bei Cyclothiazeno-Komplexen von Molybdän und Wolfram. Die Kristallstrukturen von [{Mo(N3S2)(Cl)(OtBu)2}{Mo(O)(N3S2)(OtBu)}]2 und [W(N3S2)2(LiCl){N≡W(NPPh3)3}2]

Dietrich

Neumüller

1999

Z. anorg. allg. Chem.

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MNE Nitrido Bridges with Transition Metal Nitrogen Multiple Bonds and E = Phosphorus, Sulfur, and Chlorine

Zeitschrift anorg allge chemie

2003

A compilation is given on new syntheses, properties, and structures of complexes with M≡N—E ↔ M=N=E nitrido bridges with transition metal nitrogen multiple bonds and participation of the main group elements E of phosporus, sulfur, and chlorine.1. MNP: This atomic sequence is realized in phosphoraneiminato complexes with transition metals in high oxidation states and termal bond of the (NPR3—) ligand. A series of new complexes of this type is reported with M = zirconium, hafnium, molybdenum, tungsten, and rhenium, among these the homoleptic species [Hf(NPPh3)4] and [M(NPPh3)4]2+ with M = Mo and W. Therefrom the isolobal complexes [:N≡Mo(NPPh3)3], [:O≡W(NPPh3)3]+, [(O)2Mo(NPPh3)2], and [(O)3Re(NPPh3)] are derived.2. MNS: Adding to compounds with this atomic sequence, new complexes were developed on the basis of the functional ligand groups thionitrosyl (a), dinitridosulphate(II) (b), dinitridosulphate(IV) (c), and cyclothiazeno (d) (cyclo‐3, 5‐dithia‐2, 4, 6‐triazino):magnified image3. MNCl: Novel N‐chloroimido complexes of tungsten are described. [F4W≡N—Cl]4, which is tetrameric according to the IR spectrum, was obtained by direct fluorination from [Cl4W≡N—Cl]2 or, surprisingly, from W(N)Cl3. With acetonitrile the monomeric molecular complex [CH3CN→WF4(≡N—Cl)] is formed. In an unexpected pathway K[F5W≡N—Cl] was obtained from a redox reaction of W(N)Cl3 with trimethylstannyl fluoride in the presence of potassium fluoride. The ionic compound forms double layers with short Cl···F contacts.

IR‐Spektren ¹⁵N‐isotopenmarkierter Nitrido‐, Chlorthionitreno‐ und Cyclothiazeno‐Komplexe von Molybdän, Wolfram und Rhenium

Dietrich

Zeitschrift anorg allge chemie

2007

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The IR spectra of selected, 15 N labelled complexes of molybdenum, tungsten, and rhenium with metal-nitrogen multiple bonds are reported. The examined compounds include nitrido complexes (I), chlorothionitreno complexes (II), and cyclo-thiazeno complexes (III): The results of IR spectroscopy allow reliable assignments of characteristic vibrational modes for the types I and II, whereas the assignments of vibrational modes of compounds of type III are influenced by MN 3 S 2 ring vibrations.