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PPh 4 {MoNCI 3 [N(SiMe 3 ) 2 ]}, ein Nitrido‐Amido‐Komplex von MoIybdän(VI)
Author(s) -
Fenske D.,
Frankenau A.,
Dehnicke K.
Publication year - 1989
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.655740103
Subject(s) - chemistry , trimethylsilyl , crystal structure , molybdenum , stereochemistry , tetragonal crystal system , crystallography , dichloromethane , triclinic crystal system , octahedron , x ray crystallography , tris , medicinal chemistry , inorganic chemistry , solvent , organic chemistry , biochemistry , physics , diffraction , optics
Inhaltsübersicht. PPh 4 {MoNCl 3 [N(SiMe 3 ) 2 ]} entsteht aus PPh 4 [MoNCl 4 ] und N,N,N′‐Tris‐(trimethylsilyl)benzamidin in siedendem Dichlormethan in Form bernsteinfarbener Kristalle, die wir IR‐spektroskopisch und durch eine röntgenographische Strukturanalyse charakterisiert haben. Raumgruppe P2 1 /n, Z = 4, R = 4,3% für 5168 unabhängige beobachtete Reflexe. Die Gitterkonstanten betragen für −65°C: A = 918,9; b = 2850,5; c = 1353,9 pm; β = 107,51°. Die Verbindung besteht aus PPh 4 + ‐Ionen und Anionen [MoNCl 3 [N(SiMe 3 ) 2 ]} – , in denen das Molybdänatom verzerrt tetragonal‐pyramidal von dem Nitridoliganden in Apical‐Position (r MoN = 165 pm), von drei Chloratomen und von dem N‐Atom des Bis(trimethylsilyl)amido‐Liganden (r MoN = 194 pm) umgeben ist. Das N‐Atom des Amido‐Liganden besitzt eine planare Umgebung. PPh 4 {MoNCl 3 [N(SiMe 3 ) 2 ]}, a Nitrido Amido Complex of Molybdenum (VI) PPh 4 {MoNCl 3 [N(SiMe 3 ) 2 }] has been prepared by the reaction of PPh 4 [MoNCl 4 ] with N,N,N′‐Tris(trimethylsilyl)benzamidine in boiling dichloromethane, forming amber coloured crystals, which were characterized by their IR spectrum as well as by an X‐ray structure determination. Space group P2 1 /n, Z = 4, R = 0.043 for 5168 observed independent reflexions. The lattice dimensions are at −65°C: A = 918.9; b = 2850.5; c = 1353.9 pm; β = 107.51°. The compound consists of PPh 4 + ions and anions {MoNCl 3 [N(SiMe 3 ) 2 ]} – in which the complex molybdenum anion forms a distorted tetragonal pyramid with the nitrido ligand (r MoN 165 pm) in the apical position and the chlorine atoms along with the nitrogen atom of the amido ligand (r MoN 194 pm) in the basical positions. The N atom of the amido ligand has a planar geometry.