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Synthese und Kristallstruktur des Nitrido-Oxalato-Osmats PPh4{Na(15-Krone-5)[OsNCl3(C2O4)]} (1993)

Buth, Silke ; Harms, Klaus ; Dehnicke, Kurt

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 619 (1993), S. 1409-1413

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ISSN: 0044-2313

Keywords: Nitrido Oxalato Complex of Osmium ; Synthesis ; NMR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Synthesis and Crystal Structure of the Nitrido Oxalato Osmate PPh4{Na(15-Crown-5)[OsNCl3(C2O4)]}The title compound has been prepared by slow reaction of PPh4[OsNCl4] with sodium oxalate in boiling dichloromethane in the presence of 15-crown-5, forming violet crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 4 769 observed unique reflections, R = 0.035. Lattice dimensions at -80°C: a = 1 931.4, b = 1 178.7, c = 1 764.1 pm, β = 99.39°. The structure consists of PPh4+ ions and ion pairs {Na(15-crown-5)[OsNCl3(C2O4)]}-, in which the osmium atom is distortedly octahedrally coordinated by the nitrido ligand, by three chlorine atoms, and by two oxygen atoms of the oxalato group. The remaining oxygen atoms of the oxalato ligand are coordinated to the sodium atom, which, together with the five oxygen atoms of the crown ether molecule, gets coordination number seven.

Notes: Die Titelverbindung entsteht in langsamer Reaktion aus PPh4[OsNCl4] und Natriumoxalat in Gegenwart von 15-Krone-5 in siedendem Dichlormethan. Die tiefvioletten Kristalle wurden durch eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, Strukturlösung mit 4 769 beobachteten unabhängigen Reflexen, R = 0,035. Gitterkonstanten bei -80°C: a = 1 931,4; b = 1 178,7; c = 1 764,1 pm; β = 99,39°. Die Struktur besteht aus PPh4+-Ionen und Ionenpaaren {Na(15-Krone-5)[OsNCl3(C2O4)]}-, in denen das Osmiumatom verzerrt oktaedrisch von einem terminalen Nitridoliganden, von drei Chloratomen und von zwei Sauerstoffatomen der Oxalatogruppe koordiniert ist. Die beiden übrigen O-Atome der Oxalatogruppe sind mit dem Natriumion koordiniert, so daß dieses zusammen mit den Sauerstoffatomen des Kronenethers die Koordinationszahl sieben erreicht.

Additional Material: 2 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19936190815

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Synthese und Kristallstrukturen der Nitridodiolato-Osmate(VI) PPh4[OsNCl2(O2C2H4)] und PPh4[OsNCl2(O2C2Me4)] · 2 THF (1993)

Buth, Silke ; Harms, Klaus ; König, Peter ; [et al.]

Weinheim : Wiley-Blackwell

Zeitschrift für anorganische Chemie 619 (1993), S. 853-858

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ISSN: 0044-2313

Keywords: Nitrido Diolato Osmates(VI) ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Syntheses and Crystal Structures of the Nitridodiolato Osmates(VI) PPh4[OsNCl2(O2C2H4)] and PPh4[OsNCl2(O2C2Me4)] · 2 THFThe title compounds were prepared by the reaction of PPh4[OsNCl4] with glycole and pinacole, respectively, in CH2Cl2 and THF, respectively, in the presence of triethylamine, forming orange-red single crystals. According to the crystal structure determinations the compounds have ionic structures. In the anions the nitrido ligand occupies the apical position of the distorted tetragonal pyramid, and the two chlorine atoms and the two oxygen atoms of the diolato ligands are in equatorial positions.PPh4[OsNCl2(O2C2H4)]: Space group P21/n, Z = 4, 3 331 observed unique reflections, R = 0.031. Lattice dimensions at 19°C: a = 1 750.3, b = 816.8, c = 1 816.5 pm, β = 95.16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Space group P1, Z = 2, 5 238 observed unique reflections, R = 0.051. Lattice dimensions at -80°C: a = 898.9, b = 1 405.1, c = 1 518.6 pm, α = 93.66°, β = 92.89°, γ = 92.51°.

Notes: Die Titelverbindungen entstehen als orangefarbene Einkristalle bei Reaktionen von PPh4[OsNCl4] mit Glykol bzw. mit Pinakol in Dichlormethan bzw. in Tetrahydrofuran in Gegenwart von Triethylamin. Nach den Ergebnissen der Kristallstrukturanalysen haben die Verbindungen ionischen Aufbau. In den Anionen sind die Osmiumatome verzerrt tetragonal von dem Nitridoliganden in der Apicalposition und von zwei Chloratomen und von den zwei Sauerstoffatomen der chelatisierenden Diolatoliganden in den Äquatorialpositionen umgeben.PPh4[OsNCl2(O2C2H4)]: Raumgruppe P21/n, Z = 4, 3 331 beobachtete unabhängige Reflexe, R = 3,1%. Gitterkonstanten bei 19°C: a = 1 750,3; b = 816,8; c = 1 816,5 pm; β = 95,16°.PPh4[OsNCl2(O2C2Me4)] · 2 THF: Raumgruppe P1, Z = 2, 5 238 beobachtete unabhängige Reflexe, R = 5,1%. Gitterkonstanten bei -80°C: a = 898,9; b = 1 405,1; c = 1 518,6 pm; α = 93,66°; β = 92,89°; γ = 92,51°.

Additional Material: 4 Ill.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1002/zaac.19936190508

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